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ECSS-E-HB-32-20 Part 4A

20 March 2011

Space engineering
Structural materials handbook Part 4: Integrity control, verification
guidelines and manufacturing
NOTE:
Thispdffiledoesnotcontainautomaticcrossreferences.Tomakeuseof
thecrossreferencespleaseusetheMSWordversionofthisdocument.

ECSS Secretariat
ESA-ESTEC
Requirements & Standards Division
Noordwijk, The Netherlands

ECSSEHB3220Part4A
20March2011

Foreword
ThisHandbookisonedocumentoftheseriesofECSSDocumentsintendedtobeusedassupporting
materialforECSSStandardsinspaceprojectsandapplications.ECSSisacooperativeeffortofthe
European Space Agency, national space agencies and European industry associations for the
purposeofdevelopingandmaintainingcommonstandards.
ThishandbookhasbeenpreparedbytheECSSEHB3230WorkingGroup,reviewedbytheECSS
ExecutiveSecretariatandapprovedbytheECSSTechnicalAuthority.

Disclaimer
ECSS does not provide any warranty whatsoever, whether expressed, implied, or statutory,
including,butnotlimitedto,anywarrantyofmerchantabilityorfitnessforaparticularpurposeor
anywarrantythatthecontentsoftheitemareerrorfree.InnorespectshallECSSincuranyliability
for any damages, including, but not limited to, direct, indirect, special, or consequential damages
arisingoutof,resultingfrom,orinanywayconnectedtotheuseofthisdocument,whetherornot
baseduponwarranty,businessagreement,tort,orotherwise;whetherornotinjurywassustained
bypersonsorpropertyorotherwise;andwhetherornotlosswassustainedfrom,oraroseoutof,
theresultsof,theitem,oranyservicesthatmaybeprovidedbyECSS.

Publishedby:

Copyright:

ESARequirementsandStandardsDivision
ESTEC,P.O.Box299,
2200AGNoordwijk
TheNetherlands
2011bytheEuropeanSpaceAgencyforthemembersofECSS

ECSSEHB3220Part4A
20March2011

Change log

ECSSEHB3220Part4A

Firstissue

20March2011

ECSSEHB3220Part4A
20March2011

Table of contents
Change log .................................................................................................................3
Introduction..............................................................................................................28
33 Aspects of damage tolerance............................................................................29
33.1 Introduction............................................................................................................... 29
33.1.1

Damage tolerance ...................................................................................... 29

33.1.2

Damage events .......................................................................................... 29

33.1.3

Damage tolerance criteria .......................................................................... 29

33.2 General guidelines ................................................................................................... 30


33.2.1

Fracture control .......................................................................................... 30

33.2.2

Durability..................................................................................................... 30

33.2.3

Damage ...................................................................................................... 30

33.2.4

Defects in composites ................................................................................ 30

33.2.5

Impact damage........................................................................................... 33

33.3 Damage tolerance criteria ........................................................................................ 34


33.3.1

General....................................................................................................... 34

33.3.2

Load paths.................................................................................................. 35

33.3.3

Environment ............................................................................................... 35

33.3.4

Damage ...................................................................................................... 35

33.3.5

Residual strength........................................................................................ 36

33.3.6

Safe-life ...................................................................................................... 36

33.3.7

Fail-safe...................................................................................................... 36

33.3.8

Stiffness...................................................................................................... 36

33.3.9

Loads.......................................................................................................... 36

33.3.10 Environmental factors................................................................................. 36


33.3.11 Inspection ................................................................................................... 36
33.3.12 Summary .................................................................................................... 37
33.4 Defect standardisation.............................................................................................. 37
33.4.1

General....................................................................................................... 37

33.4.2

Types of defects ......................................................................................... 38

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33.5 Effect of macroscopic defects on static load ............................................................ 40
33.5.1

Composite failure........................................................................................ 40

33.5.2

Use of fracture mechanics.......................................................................... 40

33.5.3

Multi-angle laminates.................................................................................. 40

33.6 Test and analysis ..................................................................................................... 41


33.6.1

General....................................................................................................... 41

33.6.2

Constituent tests......................................................................................... 43

33.6.3

Lamina tests ............................................................................................... 44

33.6.4

Laminate tests ............................................................................................ 44

33.6.5

Structural element and component tests .................................................... 44

33.6.6

Structural sub-component or full-scale tests .............................................. 44

33.6.7

Delamination............................................................................................... 44

33.7 Other features of damage-tolerance design ............................................................. 46


33.7.1

Acoustic fatigue .......................................................................................... 46

33.7.2

Proof testing ............................................................................................... 46

33.7.3

Metallic parts .............................................................................................. 46

33.7.4

Thermal and meteoroid protection system ................................................. 46

33.7.5

Impact dynamics crashworthiness........................................................... 46

33.7.6

Flammability, toxicity and off-gassing......................................................... 46

33.7.7

Lightning protection .................................................................................... 47

33.8 Improving damage tolerance with higher toughness laminates................................ 47


33.8.1

General....................................................................................................... 47

33.8.2

Material-related aspects ............................................................................. 47

33.8.3

Lay-up aspects ........................................................................................... 48

33.9 References ............................................................................................................... 48


33.9.1

General....................................................................................................... 48

33.9.2

ECSS documents ....................................................................................... 49

33.9.3

MIL standards............................................................................................. 49

34 Inspection and quality assurance .....................................................................50


34.1 Introduction............................................................................................................... 50
34.2 Fabrication and quality assurance............................................................................ 50
34.2.1

Quality assurance....................................................................................... 50

34.3 Inspection, maintenance and repair ......................................................................... 51


34.3.1

Inspection and maintenance....................................................................... 51

34.3.2

Repairs ....................................................................................................... 52

34.4 Inspection ................................................................................................................. 52


34.4.1

Basic considerations................................................................................... 52

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34.5 Definition of inspection procedures .......................................................................... 53
34.5.1

Procedures ................................................................................................. 53

34.5.2

Thin composite laminates........................................................................... 54

34.5.3

Thick composite laminates ......................................................................... 54

34.6 Non-destructive inspection techniques..................................................................... 55


34.6.1

Introduction................................................................................................. 55

34.6.2

Damage tolerant designs............................................................................ 55

34.6.3

Advances in NDT........................................................................................ 55

34.6.4

Techniques ................................................................................................. 56

34.6.5

Smart technologies for condition monitoring .............................................. 57

34.7 Defects and anomalies for detection ........................................................................ 57


34.7.1

General....................................................................................................... 57

34.7.2

Emphasis of NDT development.................................................................. 58

34.8 Overview of NDT techniques.................................................................................... 58


34.8.1

Selection of NDT technique........................................................................ 58

34.8.2

Detection of defects.................................................................................... 59

34.9 Traditional contact NDT techniques ......................................................................... 65


34.9.1

General....................................................................................................... 65

34.9.2

Visual inspection......................................................................................... 65

34.9.3

Dye penetrant ............................................................................................. 65

34.9.4

Magnetic particle ........................................................................................ 65

34.9.5

Mechanical resonance or impedance......................................................... 65

34.10 Ultrasonic techniques ............................................................................................... 66


34.10.1 Introduction................................................................................................. 66
34.10.2 Modes of examination ................................................................................ 67
34.10.3 Ultrasonic signal presentation .................................................................... 67
34.10.4 Data and image processing........................................................................ 67
34.10.5 Equipment calibration ................................................................................. 68
34.10.6 Large area scanning................................................................................... 69
34.10.7 Acousto-ultrasonics .................................................................................... 69
34.10.8 Lamb wave (guided wave).......................................................................... 70
34.10.9 Rayleigh wave techniques.......................................................................... 71
34.10.10

Backscattering techniques............................................................ 71

34.10.11

Transducer technology ................................................................. 72

34.10.12

Air-coupled techniques (non-contact)........................................... 75

34.11 Acoustic emission..................................................................................................... 78


34.12 Laser ultrasonics ...................................................................................................... 79

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34.12.1 General....................................................................................................... 79
34.12.2 Basic principles........................................................................................... 80
34.13 Holography ............................................................................................................... 81
34.13.1 Introduction................................................................................................. 81
34.13.2 Laser interferometric techniques ................................................................ 82
34.13.3 Vibration, pressure and thermal loading..................................................... 83
34.13.4 Electronic imaging ...................................................................................... 83
34.13.5 Examination of space structures ................................................................ 84
34.14 Laser shearography ................................................................................................. 85
34.14.1 Introduction................................................................................................. 85
34.14.2 Basic technique .......................................................................................... 85
34.14.3 Characteristics of shearography................................................................. 86
34.15 Thermography .......................................................................................................... 87
34.15.1 Introduction................................................................................................. 87
34.15.2 Techniques ................................................................................................. 88
34.15.3 Heat sources and pulse duration................................................................ 92
34.15.4 Detection capabilities.................................................................................. 92
34.15.5 Limitations of thermography ....................................................................... 93
34.16 X-ray radiography..................................................................................................... 94
34.16.1 Introduction................................................................................................. 94
34.16.2 X-ray techniques......................................................................................... 95
34.16.3 Digital radiographic system developments ................................................. 96
34.16.4 Defect resolution......................................................................................... 99
34.17 Computer tomography.............................................................................................. 99
34.17.1 Introduction................................................................................................. 99
34.17.2 Basic technique .......................................................................................... 99
34.17.3 Attributes of CT scanning ......................................................................... 100
34.17.4 Micro-tomography..................................................................................... 101
34.18 Eddy currents ......................................................................................................... 101
34.18.1 Introduction............................................................................................... 101
34.18.2 Developments in eddy current techniques ............................................... 102
34.19 Other NDT techniques............................................................................................ 103
34.19.1 General..................................................................................................... 103
34.19.2 Microwave ................................................................................................ 104
34.19.3 Heat and photosensitive agents ............................................................... 104
34.19.4 Electrical impedance ................................................................................ 104
34.19.5 Acoustic microscopy................................................................................. 104

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34.19.6 Nuclear magnetic resonance (NMR) ........................................................ 105
34.19.7 Neutron radiography................................................................................. 105
34.19.8 Gamma radiography................................................................................. 105
34.19.9 D sight - Diffracto sight ............................................................................. 105
34.20 NDT for adhesive bond defects .............................................................................. 106
34.20.1 General..................................................................................................... 106
34.20.2 Disbonds, voids and porosity.................................................................... 106
34.20.3 Cohesion and adhesion............................................................................ 107
34.21 NDT for space applications .................................................................................... 107
34.21.1 Introduction............................................................................................... 107
34.21.2 Developments in inspection...................................................................... 108
34.21.3 Summary of NDT techniques ................................................................... 108
34.22 Rupture tests .......................................................................................................... 110
34.22.1 Application ................................................................................................ 110
34.23 Test related items ................................................................................................... 111
34.23.1 General..................................................................................................... 111
34.23.2 Major items ............................................................................................... 111
34.23.3 Qualification tests ..................................................................................... 112
34.24 Structural test reports ............................................................................................. 123
34.25 Analysis and test documents.................................................................................. 124
34.26 References ............................................................................................................. 126
34.26.1 General..................................................................................................... 126
34.26.2 ECSS documents ..................................................................................... 138

35 Objective of verification ...................................................................................139


35.1 Introduction............................................................................................................. 139
35.1.1

General..................................................................................................... 139

35.1.2

Composite structures................................................................................ 139

35.1.3

Composite materials................................................................................. 139

36 Procurement specifications for raw materials ...............................................141


36.1 Introduction............................................................................................................. 141
36.1.1

Guidelines................................................................................................. 141

36.2 Specification methods ............................................................................................ 141


36.2.1

Fiche sheet principle................................................................................. 141

36.2.2

Specific material specification .................................................................. 142

36.3 Guidelines on resin procurement ........................................................................... 142


36.3.1

Scope ....................................................................................................... 142

36.3.2

Basic information to be provided by the supplier...................................... 143


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36.4 Guidelines on carbon and other fibre prepreg procurement................................... 147
36.4.1

Scope ....................................................................................................... 147

36.4.2

Description and classification of prepreg.................................................. 147

36.4.3

Prepreg charachteristics for qualification and batch testing ..................... 148

36.4.4

Laminate Characteristics .......................................................................... 151

36.4.5

Test methods............................................................................................ 152

36.5 References ............................................................................................................. 153


36.5.1

ECSS documents ..................................................................................... 153

36.5.2

ESA publications ...................................................................................... 153

37 Philosophy of assessment of design allowables ..........................................154


37.1 Introduction............................................................................................................. 154
37.2 Carbon fibre reinforced plastics.............................................................................. 154
37.2.1

Design values ........................................................................................... 154

37.3 Definition of design allowables ............................................................................... 155


37.3.1

'A' basis allowable .................................................................................... 155

37.3.2

'B' basis allowable .................................................................................... 155

37.4 Development procedure ......................................................................................... 155


37.5 Test data ................................................................................................................ 155
37.5.1

Material..................................................................................................... 155

37.5.2

Data .......................................................................................................... 156

37.6 References ............................................................................................................. 160


37.6.1

General..................................................................................................... 160

38 Manufacturing techniques ...............................................................................161


38.1 Introduction............................................................................................................. 161
38.1.1

Processing techniques ............................................................................. 161

38.1.2

Process selection ..................................................................................... 161

38.2 Process selection criteria ....................................................................................... 162


38.3 Hand lay-up ............................................................................................................ 162
38.3.1

General..................................................................................................... 162

38.3.2

Wet lamination.......................................................................................... 163

38.3.3

Prepreg lay-up .......................................................................................... 166

38.4 Autoclave moulding ................................................................................................ 170


38.4.1

Use ........................................................................................................... 170

38.4.2

Basic process ........................................................................................... 170

38.4.3

Bag moulding methods............................................................................. 171

38.4.4

Features of bag moulding......................................................................... 174

38.4.5

Bagging techniques .................................................................................. 175


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38.4.6

Tool materials ........................................................................................... 176

38.4.7

Cure schedules......................................................................................... 178

38.5 Filament winding .................................................................................................... 179


38.5.1

Basic process ........................................................................................... 179

38.5.2

Applications .............................................................................................. 179

38.5.3

Winding process ....................................................................................... 180

38.5.4

Mandrels................................................................................................... 181

38.5.5

Sandwich constructions............................................................................ 181

38.5.6

Tape winding ............................................................................................ 182

38.6 Filament-winding machines .................................................................................... 182


38.6.1

General..................................................................................................... 182

38.6.2

Polar winding ............................................................................................ 182

38.6.3

Helical winding.......................................................................................... 184

38.7 Resin transfer moulding ......................................................................................... 185


38.7.1

General..................................................................................................... 185

38.7.2

Basic process ........................................................................................... 185

38.7.3

Applications .............................................................................................. 186

38.7.4

Fibre preforms .......................................................................................... 186

38.7.5

Resin injection .......................................................................................... 187

38.7.6

Process variables ..................................................................................... 188

38.7.7

Process advantages ................................................................................. 188

38.8 Pultrusion ............................................................................................................... 189


38.8.1

Use ........................................................................................................... 189

38.8.2

Basic process ........................................................................................... 189

38.8.3

Pull-forming .............................................................................................. 190

38.9 Table rolling............................................................................................................ 191


38.9.1

Tubular sections ....................................................................................... 191

38.10 Pressure and mechanical forming .......................................................................... 191


38.10.1 General..................................................................................................... 191
38.10.2 Fibre metal laminates ............................................................................... 191
38.10.3 Thermoplastic composites........................................................................ 192
38.11 Injection moulding .................................................................................................. 192
38.11.1 General..................................................................................................... 192
38.11.2 Short fibre composites.............................................................................. 192
38.12 Radiation curing ..................................................................................................... 193
38.12.1 Process developments ............................................................................. 193
38.12.2 EB electron beam curing .......................................................................... 194

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38.12.3 Microwave ................................................................................................ 198
38.12.4 UV curing.................................................................................................. 199
38.13 Preform technology ................................................................................................ 199
38.13.1 General..................................................................................................... 199
38.13.2 Braids ....................................................................................................... 200
38.13.3 Commingled fibre performs ...................................................................... 200
38.14 Fibre placement...................................................................................................... 201
38.14.1 Introduction............................................................................................... 201
38.14.2 Advantages............................................................................................... 204
38.14.3 Repeatability in lay-up and properties ...................................................... 205
38.14.4 Mixed materials in the same lay-up .......................................................... 206
38.14.5 Major advantages of fibre placement compared with other
technologies ............................................................................................. 207
38.14.6 Examples of European launcher and satellite structures made by
fibre placement ......................................................................................... 208
38.15 Out of autoclave ..................................................................................................... 209
38.15.1 Introduction............................................................................................... 209
38.15.2 Aerospace structural parts........................................................................ 209
38.15.3 Composite materials................................................................................. 210
38.15.4 Tooling...................................................................................................... 210
38.16 References ............................................................................................................. 211
38.16.1 General..................................................................................................... 211
38.16.2 ECSS standards ....................................................................................... 217

39 Machining techniques ......................................................................................218


39.1 Introduction............................................................................................................. 218
39.2 Basic rules.............................................................................................................. 218
39.2.1

General..................................................................................................... 218

39.2.2

Equipment ................................................................................................ 218

39.3 Routing ................................................................................................................... 219


39.3.1

Carbon/epoxy composites ........................................................................ 219

39.3.2

Aramid/epoxy composites ........................................................................ 219

39.3.3

Trimming and bevelling ............................................................................ 220

39.4 Sanding .................................................................................................................. 221


39.4.1

General..................................................................................................... 221

39.4.2

Fit or trim .................................................................................................. 221

39.4.3

Bonding .................................................................................................... 222

39.4.4

Aramid/epoxy composites ........................................................................ 223

39.5 Sawing.................................................................................................................... 223


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39.5.1

Basic rules ................................................................................................ 223

39.5.2

Bandsawing .............................................................................................. 223

39.5.3

Circular sawing ......................................................................................... 224

39.5.4

Sabre sawing............................................................................................ 225

39.6 Countersinking ....................................................................................................... 226


39.6.1

General..................................................................................................... 226

39.6.2

Carbon and glass reinforced epoxy.......................................................... 226

39.6.3

Aramid/epoxy composites ........................................................................ 226

39.7 Counterboring......................................................................................................... 227


39.8 Milling ..................................................................................................................... 228
39.8.1

Basic Rules............................................................................................... 228

39.8.2

Plunge-cut milling ..................................................................................... 228

39.9 Drilling .................................................................................................................... 229


39.9.1

Basic problems ......................................................................................... 229

39.9.2

Drill bits for composites ............................................................................ 230

39.10 Orbital drilling ......................................................................................................... 232


39.10.1 Introduction............................................................................................... 232
39.10.2 Advantages............................................................................................... 233
39.10.3 Drilling parameters ................................................................................... 233
39.10.4 Equipment ................................................................................................ 233
39.10.5 Application examples................................................................................ 234
39.11 References ............................................................................................................. 235
39.11.1 General..................................................................................................... 235
39.11.2 ECSS standards ....................................................................................... 235

40 Manufacturing costs.........................................................................................236
40.1 Introduction............................................................................................................. 236
40.2 Cost drivers ............................................................................................................ 237
40.2.1

General..................................................................................................... 237

40.2.2

Project cost drivers ................................................................................... 237

40.2.3

Mass for cost budgets .............................................................................. 237

40.2.4

Materials selection.................................................................................... 237

40.2.5

Design for manufacturing ......................................................................... 238

40.2.6

Manufacturing expertise ........................................................................... 238

40.2.7

Tooling and consumables......................................................................... 238

40.2.8

Processing times ...................................................................................... 238

40.2.9

Labour costs ............................................................................................. 239

40.2.10 Part count ................................................................................................. 239

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40.2.11 Unit numbers ............................................................................................ 239
40.2.12 Product life and sourcing .......................................................................... 240
40.3 Cost optimisation.................................................................................................... 240
40.3.1

Load-carrying structures........................................................................... 240

40.4 Cost advantages of composites ............................................................................. 245


40.4.1

Material costs ........................................................................................... 245

40.4.2

Manufacturing costs ................................................................................. 245

40.5 Satellite thrust cylinders ......................................................................................... 245


40.6 Launcher fairing cylinders ...................................................................................... 246
40.6.1

General..................................................................................................... 246

40.6.2

Potential fairing designs ........................................................................... 246

40.6.3

Selection of designs ................................................................................. 250

40.6.4

Process and material trade-off ................................................................. 251

40.7 Thermoplastic versus thermoset ............................................................................ 253


40.7.1

General..................................................................................................... 253

40.7.2

Recurring spacecraft components............................................................ 254

40.7.3

Thermoplastic composites in aircraft ........................................................ 259

40.7.4

Conclusions .............................................................................................. 261

40.8 Automation ............................................................................................................. 261


40.9 Cost analysis methods ........................................................................................... 262
40.10 References ............................................................................................................. 262
40.10.1 General..................................................................................................... 262

41 Repair of composites .......................................................................................264


41.1 Introduction............................................................................................................. 264
41.2 Damage classification ............................................................................................ 264
41.2.1

Life-histories of composite structures ....................................................... 264

41.2.2

Inspection and criticality of damage ......................................................... 264

41.2.3

Repair zones ............................................................................................ 265

41.3 Damage categories ................................................................................................ 265


41.3.1

Impact energy levels................................................................................. 265

41.3.2

Damage types .......................................................................................... 266

41.4 Basic repair concepts ............................................................................................. 269


41.4.1

General..................................................................................................... 269

41.4.2

Basic types of repairs ............................................................................... 269

41.4.3

Repair selection........................................................................................ 269

41.5 Flush repair concepts ............................................................................................. 271


41.5.1

Applications .............................................................................................. 271

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41.5.2

Post-repair properties ............................................................................... 271

41.5.3

Design ...................................................................................................... 271

41.5.4

Manufacture.............................................................................................. 271

41.6 Bonded external repair concepts............................................................................ 272


41.6.1

Applications .............................................................................................. 272

41.6.2

Post-repair properties ............................................................................... 272

41.6.3

Design ...................................................................................................... 272

41.6.4

Manufacture.............................................................................................. 273

41.7 Bolted external repair concepts .............................................................................. 273


41.7.1

Applications .............................................................................................. 273

41.7.2

Post-repair properties ............................................................................... 274

41.7.3

Design ...................................................................................................... 274

41.7.4

Manufacture.............................................................................................. 274

41.8 Sandwich structure repair concepts ....................................................................... 275


41.8.1

No core damage ....................................................................................... 275

41.8.2

Core damage............................................................................................ 275

41.8.3

Manufacture.............................................................................................. 275

41.9 References ............................................................................................................. 276


41.9.1

General..................................................................................................... 276

42 Basic characteristics of new advanced materials .........................................278


42.1 Introduction............................................................................................................. 278
42.2 Material groups....................................................................................................... 278
42.2.1

Metallic materials...................................................................................... 278

42.2.2

Ceramic materials..................................................................................... 279

42.2.3

Material classification ............................................................................... 279

42.3 Features of alloys and metal matrix composites .................................................... 281


42.3.1

Structural alloys ........................................................................................ 281

42.3.2

Properties ................................................................................................. 282

42.3.3

Material developments ............................................................................. 282

42.3.4

Effects of reinforcements.......................................................................... 283

42.3.5

Processing................................................................................................ 283

42.4 Features of ceramic and inorganic composites ...................................................... 284


42.4.1

Features ................................................................................................... 284

42.4.2

Properties ................................................................................................. 285

42.4.3

High-temperature use............................................................................... 285

42.5 High temperature and interface phenomena .......................................................... 286


42.5.1

Effects of processing temperature............................................................ 286

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42.5.2

High-temperature applications.................................................................. 287

42.6 Refractory and ceramic fibres................................................................................. 288


42.6.1

Introduction............................................................................................... 288

42.6.2

Types of refractory and ceramic fibre ....................................................... 288

42.6.3

Use in composites .................................................................................... 289

42.6.4

Thermal stability ....................................................................................... 290

42.7 References ............................................................................................................. 303


42.7.1

General..................................................................................................... 303

43 Technical ceramics ..........................................................................................305


43.1 Introduction............................................................................................................. 305
43.1.1

General..................................................................................................... 305

43.1.2

Technical ceramics for space structures .................................................. 306

43.2 Material groups....................................................................................................... 307


43.2.1

Composition.............................................................................................. 307

43.2.2

Oxides ...................................................................................................... 307

43.2.3

Carbides ................................................................................................... 309

43.2.4

Nitrides ..................................................................................................... 309

43.2.5

Elemental.................................................................................................. 311

43.2.6

Glass-ceramics......................................................................................... 313

43.2.7

Sources .................................................................................................... 313

43.3 Design aspects....................................................................................................... 315


43.3.1

Guidelines................................................................................................. 315

43.3.2

Property and performance evaluation ...................................................... 316

43.4 Processing aspects ................................................................................................ 319


43.4.1

Manufacturing processes ......................................................................... 319

43.4.2

Health and safety...................................................................................... 320

43.4.3

Green shapes ........................................................................................... 320

43.4.4

Densification ............................................................................................. 323

43.4.5

Combined shaping and densification........................................................ 323

43.4.6

Vapour-phase techniques......................................................................... 324

43.4.7

Machining ................................................................................................. 324

43.4.8

Joining ...................................................................................................... 324

43.5 Applications ............................................................................................................ 325


43.5.1

Industrial ................................................................................................... 325

43.5.2

Aerospace ................................................................................................ 326

43.5.3

Materials ................................................................................................... 327

43.6 Aluminium oxide: Alumina ...................................................................................... 331

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43.6.1

Typical characteristics .............................................................................. 331

43.6.2

Typical properties ..................................................................................... 332

43.7 Aluminium nitride.................................................................................................... 335


43.7.1

Typical characteristics .............................................................................. 335

43.7.2

Typical properties ..................................................................................... 336

43.8 Boron carbide ......................................................................................................... 338


43.8.1

Typical characteristics .............................................................................. 338

43.8.2

Typical properties ..................................................................................... 338

43.9 Boron nitride ........................................................................................................... 340


43.9.1

Typical characteristics .............................................................................. 340

43.9.2

Typical properties ..................................................................................... 341

43.9.3

Space application examples..................................................................... 342

43.10 Carbon.................................................................................................................... 344


43.10.1 Typical characteristics .............................................................................. 344
43.10.2 Typical properties ..................................................................................... 347
43.11 Silicon oxide: Silica................................................................................................. 351
43.11.1 Typical characteristics .............................................................................. 351
43.11.2 Typical properties ..................................................................................... 351
43.12 Silicon carbide ........................................................................................................ 353
43.12.1 Typical characteristics .............................................................................. 353
43.12.2 Typical properties ..................................................................................... 354
43.12.3 Materials for space applications ............................................................... 356
43.12.4 Cesic ...................................................................................................... 357
43.12.5 SiC 54S ................................................................................................... 363
43.12.6 SiC-100 ................................................................................................... 366
43.13 Silicon nitride .......................................................................................................... 378
43.13.1 Typical characteristics .............................................................................. 378
43.13.2 Typical properties ..................................................................................... 379
43.14 Zirconium oxide: Zirconia ....................................................................................... 380
43.14.1 Typical characteristics .............................................................................. 380
43.14.2 Typical properties ..................................................................................... 380
43.15 Structural glass: Glass ceramics ............................................................................ 382
43.15.1 Introduction............................................................................................... 382
43.15.2 Commercially-available glass and glass ceramics ................................... 382
43.15.3 Glass ceramics for space applications ..................................................... 387
43.15.4 ZERODUR ............................................................................................. 388
43.15.5 ZERODUR: Properties............................................................................ 390

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43.15.6 ZERODUR: Design ................................................................................ 394
43.15.7 ZERODUR: Application examples ......................................................... 401
43.15.8 ULE Ultra low expansion titanium-silicate glass .................................... 401
43.15.9 ULE: Properties...................................................................................... 402
43.15.10

ULE: Design............................................................................. 404

43.15.11

ULE: Application examples ...................................................... 404

43.16 Speciality materials ................................................................................................ 405


43.16.1 Introduction............................................................................................... 405
43.16.2 Beryllia...................................................................................................... 405
43.16.3 Sapphire ................................................................................................... 406
43.16.4 Synthetic diamond .................................................................................... 406
43.17 CVD diamond ......................................................................................................... 407
43.17.1 Introduction............................................................................................... 407
43.17.2 Typical characteristics .............................................................................. 408
43.17.3 Typical properties ..................................................................................... 408
43.17.4 Application examples................................................................................ 410
43.18 Cesic: NIRSpec optical bench .............................................................................. 414
43.18.1 Introduction............................................................................................... 414
43.18.2 Material characteristics............................................................................. 414
43.18.3 Development of optical bench .................................................................. 415
43.18.4 Conclusions .............................................................................................. 422
43.19 Zerodur: Applications case study.......................................................................... 422
43.19.1 Introduction............................................................................................... 422
43.19.2 Terrestrial mirrors ..................................................................................... 423
43.19.3 Optical bench............................................................................................ 423
43.20 References ............................................................................................................. 424
43.20.1 General..................................................................................................... 424
43.20.2 Sources .................................................................................................... 432
43.20.3 ECSS documents ..................................................................................... 432
43.20.4 Other standards........................................................................................ 432

44 Magnesium alloys and their composites........................................................433


44.1 Introduction............................................................................................................. 433
44.1.1

General..................................................................................................... 433

44.1.2

Features ................................................................................................... 433

44.1.3

Alloy classification .................................................................................... 433

44.1.4

Environmental aspects ............................................................................. 435

44.1.5

Machining ................................................................................................. 435

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44.1.6

MMC - metal matrix composites ............................................................... 436

44.1.7

Material availability ................................................................................... 436

44.1.8

Future developments................................................................................ 437

44.2 Magnesium alloys................................................................................................... 437


44.2.1

Chemical composition .............................................................................. 437

44.2.2

Mechanical properties .............................................................................. 440

44.3 Discontinuously reinforced magnesium composites............................................... 446


44.3.1

Types of discontinuous reinforcement...................................................... 446

44.3.2

Effect of particulate additions ................................................................... 447

44.3.3

Processing................................................................................................ 447

44.3.4

Properties ................................................................................................. 447

44.4 Continuously reinforced magnesium composites ................................................... 448


44.4.1

Types of composite .................................................................................. 448

44.4.2

Features ................................................................................................... 449

44.4.3

Processing................................................................................................ 449

44.4.4

Properties ................................................................................................. 449

44.4.5

Environmental resistance ......................................................................... 450

44.5 Potential applications ............................................................................................. 451


44.5.1

Alloys ........................................................................................................ 451

44.5.2

Composites............................................................................................... 451

44.5.3

Space ....................................................................................................... 451

44.6 References ............................................................................................................. 453


44.6.1

General..................................................................................................... 453

44.6.2

Sources .................................................................................................... 455

44.6.3

Organisations ........................................................................................... 455

44.6.4

ECSS standards ....................................................................................... 456

44.6.5

ASTM standards....................................................................................... 456

45 Copper alloys and their composites ...............................................................457


45.1 Introduction............................................................................................................. 457
45.2 Copper alloys ......................................................................................................... 457
45.2.1

Precipitation hardening............................................................................. 457

45.3 Copper ODS alloys................................................................................................. 458


45.3.1

Types and effects of dispersions .............................................................. 458

45.3.2

Properties ................................................................................................. 458

45.4 Discontinuously reinforced copper composites ...................................................... 460


45.4.1

General..................................................................................................... 460

45.4.2

Problems .................................................................................................. 460

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45.5 Continuously reinforced copper composites .......................................................... 461
45.5.1

General..................................................................................................... 461

45.5.2

Types and effects of reinforcements ........................................................ 461

45.5.3

Properties ................................................................................................. 461

45.6 Potential applications ............................................................................................. 462


45.7 References ............................................................................................................. 462
45.7.1

General..................................................................................................... 462

Figures
Figure 33.2-1 Summary: Defects in composite materials.................................................... 32
Figure 33.4-1 - Metal structures: Idealisation of a volumetric defect...................................... 38
Figure 33.4-2 - Composite structures: Idealisation of defects by standard circular
defect ................................................................................................................... 39
Figure 33.6-1 - Building block approach: Test programme development............................... 42
Figure 33.6-2 - Building block approach: Composite materials.............................................. 43
Figure 34.10-1 - Leaky-Lamb-wave technique for composites .............................................. 71
Figure 34.10-2 - Detection of fibre orientation by backscattering measurement .................... 72
Figure 34.10-3 Phased-array transducers: Element configurations .................................... 73
Figure 34.10-4 Phased-array transducers: Functionality .................................................... 74
Figure 34.10-5 - Non-contact ultrasonics: Air-coupled sensor configurations........................ 76
Figure 34.10-6 - Non-contact ultrasonics: Capacitive sensors in plate wave
configuration set-up ............................................................................................. 77
Figure 34.10-7 Airscan (air-coupled ultrasonics) system: Non-contact NDI of
Fokker solar panel substrates.............................................................................. 78
Figure 34.12-1 - Laser ultrasonic test system: Diagrammatic representation ........................ 80
Figure 34.13-1 - Holography by electronic imaging with random vibration excitation ............ 84
Figure 34.14-1 - Electronic shearographic system: Schematic diagram ................................ 85
Figure 34.15-1 - Basic thermographic technique ................................................................... 88
Figure 34.15-2 - Thermal-wave imaging: Photo-optical detection.......................................... 90
Figure 34.15-3 - Thermal-wave imaging: Photothermal and piezoelectric detection ............. 91
Figure 34.15-4 - Thermal-wave imaging: Photoacoustic gas cell........................................... 91
Figure 34.16-1 - Typical digital radiography systems............................................................. 97
Figure 34.17-1 - Computer tomography facility .................................................................... 100
Figure 34.19-1 - D sight - Diffracto sight schematic ............................................................. 106
Figure 37.5-1 - Probability of exceedance: Tensile strength 0............................................ 157
Figure 37.5-2 - Probability of exceedance: Tensile strength 90.......................................... 158
Figure 37.5-3 - Probability of exceedance: Compressive strength 90 ................................ 159
Figure 37.5-4 - Probability of exceedance: Interlaminar shear strength............................... 160

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Figure 38.3-1 - Hand lay-up process for mat or cloth........................................................... 163
Figure 38.3-2 - Prepreg: Direct lay-up.................................................................................. 167
Figure 38.3-3 - Prepreg: Indirect lay-up ............................................................................... 167
Figure 38.4-1 - Vacuum bag moulding method, with vertical bleeder .................................. 172
Figure 38.4-2 - Pressure bag moulding................................................................................ 172
Figure 38.4-3 - Pressure bag moulding: Press modifications............................................... 173
Figure 38.4-4 - Autoclave moulding method, with vertical bleeder....................................... 173
Figure 38.4-5 - Bag moulding: Edge bleed out system ........................................................ 176
Figure 38.4-6 - Typical cure schedule for autoclaved prepregs ........................................... 178
Figure 38.5-1 - Filament winding: Impregnation of fibres ..................................................... 180
Figure 38.6-1 - Filament winding: Polar vertical ................................................................... 183
Figure 38.6-2 - Filament winding: Polar horizontal............................................................... 183
Figure 38.6-3 - Filament winding: Polar tumbling................................................................. 184
Figure 38.6-4 - Filament winding: Helical ............................................................................. 184
Figure 38.7-1 - Resin transfer moulding (RTM): Process..................................................... 185
Figure 38.8-1 - Pultrusion: Basic process ............................................................................ 190
Figure 38.12-1 EB curing: Examples of parts and structures............................................ 197
Figure 38.13-1 - Preform technology: Architecture of woven commingled AS4/PEEK
150g 0/90 ........................................................................................................ 201
Figure 38.14-1 Fibre placement: Schematic view of the system....................................... 202
Figure 38.14-2 Fibre placement: Head.............................................................................. 203
Figure 38.14-3 Fibre placement: General view of working area........................................ 203
Figure 38.14-4 Fibre placement: Complex curvature ........................................................ 204
Figure 38.14-5 Fibre placement: Specific orientations ...................................................... 205
Figure 38.14-6 Fibre placement: Complex trajectories ..................................................... 206
Figure 38.14-7 Fibre placement: Variation of band width.................................................. 206
Figure 38.14-8 Fibre placement: Mixed-material lay-up.................................................... 207
Figure 39.3-1 - Router: Opposed helix for aramid/epoxy ..................................................... 220
Figure 39.3-2 - Router for trimming aramid/epoxy composites ............................................ 221
Figure 39.4-1 - Sanding of composites ................................................................................ 222
Figure 39.5-1 - Reverse bandsawing aramid/epoxy laminates ............................................ 224
Figure 39.5-2 - Circular sawing: Feed rate versus thickness of composite materials .......... 225
Figure 39.5-3 - Sabre sawing: Alternating tooth blade for aramid/epoxy ............................. 226
Figure 39.6-1 - Countersink for aramid/epoxy composite .................................................... 227
Figure 39.8-1 - Proper milling technique .............................................................................. 228
Figure 39.9-1 - Drill bits for composites................................................................................ 230
Figure 39.9-2 - Daggar drill in hand feed units ..................................................................... 232
Figure 39.10-1 Orbital drilling principle.............................................................................. 232
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Figure 39.10-2 Orbital drilling: Equipment mounted on a jig ............................................. 233
Figure 39.10-3 Orbital drilling: Application examples ........................................................ 234
Figure 40.3-1 - Mass/cost sensitivity for central thrust structure .......................................... 242
Figure 40.3-2 - Mass/cost sensitivity for complete structure ................................................ 243
Figure 40.3-3 - Mass to cost envelope for material improvements ...................................... 244
Figure 40.6-1 - Candidate fairing and intertank constructions.............................................. 247
Figure 40.6-2 - Fairing cylinder costs for different designs (life cycle costs per unit)........... 248
Figure 40.6-3 - Launcher fairing cylinder: Kepner-Tregoe evaluation scores for the
section designs .................................................................................................. 250
Figure 40.6-4 - Launcher fairing: Unit life cycle costs for sandwich fairing cylinder
designs for different fabrication processes ........................................................ 252
Figure 40.6-5 - Launcher fairing: Kepner-Tregoe evaluation scores for processes to
fabricate the monocoque and sandwich cylinder............................................... 253
Figure 40.7-1 - Thermoplastic components: Manufacturing unit costs as a function of
production volumes............................................................................................ 257
Figure 40.7-2 - Relative part costs for thermoplastic aircraft components: Dornier 328
landing flap rib ................................................................................................... 260
Figure 41.3-1 - Damage categories: Scratch ....................................................................... 266
Figure 41.3-2 - Damage categories: Notch .......................................................................... 266
Figure 41.3-3 - Damage categories: Chipping ..................................................................... 267
Figure 41.3-4 - Damage categories: Debonding .................................................................. 267
Figure 41.3-5 - Damage categories: Delamination............................................................... 268
Figure 41.3-6 - Damage categories: Perforation .................................................................. 268
Figure 41.4-1 - Basic repair concepts .................................................................................. 270
Figure 41.5-1 - Typical flush repair....................................................................................... 271
Figure 41.5-2 - Flush repair, used by Airbus Industrie ......................................................... 272
Figure 41.5-3 - Flush repair with adhesive film and cover plies ........................................... 272
Figure 41.6-1 - External repair: Pre-cured patches .............................................................. 273
Figure 41.6-2 - External repair: Cured in place .................................................................... 273
Figure 41.7-1 - Bolted and bonded repair using a composite patch..................................... 274
Figure 41.8-1 - Sandwich repair ........................................................................................... 276
Figure 42.2-1 - Classification of advanced metallic and ceramic materials with
temperature ....................................................................................................... 280
Figure 42.2-2 - Specific strength against temperature for advanced materials.................... 281
Figure 42.6-1 - SiC Nicalon fibre tensile strength at elevated temperature.......................... 293
Figure 42.6-2 - SiC Nicalon standard grade fibre tensile strength at elevated
temperature ....................................................................................................... 294
Figure 42.6-3 - SiC Nicalon ceramic grade fibre: tensile strength at elevated
temperature ....................................................................................................... 295

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Figure 42.6-4 - SiC Nicalon fibre: tensile strength after high temperature exposure in
air....................................................................................................................... 296
Figure 42.6-5 - SiC Nicalon fibre: tensile strength after high temperature exposure in
argon.................................................................................................................. 296
Figure 42.6-6 - SiC fibres Nicalon and Tyranno: tensile strength at elevated
temperature ....................................................................................................... 297
Figure 42.6-7 - SiC fibres Nicalon and Tyranno: modulus at elevated temperature ............ 298
Figure 42.6-8 - Alumina fibres: tensile strength at elevated temperature............................. 298
Figure 42.6-9 - Alumina fibres: modulus at elevated temperature ....................................... 299
Figure 42.6-10 - Alumina fibres: tensile strength against exposure to elevated
temperature ....................................................................................................... 299
Figure 42.6-11 - Alumina fibres: tensile strength against exposure time ............................. 300
Figure 42.6-12 - Alumina-boria-silica single filament: tensile strength at elevated
temperature in air............................................................................................... 300
Figure 42.6-13 - Alumina-boria-silica single filament: tensile modulus at elevated
temperature in air............................................................................................... 301
Figure 42.6-14 - Modulus for various fibres and matrix materials ........................................ 302
Figure 42.6-15 - Coefficients of thermal expansion for various fibres and matrix
materials ............................................................................................................ 303
Figure 43.4-1 Technical ceramics: Manufacturing processes ........................................... 320
Figure 43.9-1 Technical ceramics: pyrolitic boron nitride structure ................................ 341
Figure 43.12-1 Cesic: Basic processing sequence.......................................................... 358
Figure 43.12-2 Cesic: Silicon-infiltration processing equipment ..................................... 359
Figure 43.12-3 Cesic: Coefficient of thermal expansion ................................................. 361
Figure 43.12-4 Cesic ceramic: Example of integrally-stiffened panel............................. 362
Figure 43.12-5 SiC 54S ceramic: Process sequence ..................................................... 363
Figure 43.12-6 SiC 54S: NIRSpec prototype mirror ....................................................... 366
Figure 43.12-7 SiC-100: Production process - schematic for Herschel primary
mirror ................................................................................................................. 368
Figure 43.12-8 SiC-100: 1m diameter Demonstration Mirror ready to polish.............. 373
Figure 43.12-9 SiC-100: 1m diameter Demonstration Mirror green part joining
by ceramic bonding............................................................................................ 374
Figure 43.12-10 SiC-100: 1.35 m diameter HERSCHEL Demonstrator Breadboard
before and after brazing.................................................................................. 374
Figure 43.12-11 SiC-100: 3.5 m diameter HERSCHEL Primary Mirror
manufactured by brazing 12 SiC segments ....................................................... 375
Figure 43.12-12 SiC-100: 3.5 m diameter HERSCHEL Primary Mirror after
assembly............................................................................................................ 376
Figure 43.12-13 SiC-100: NIRSpec Optical Bench Breadboard...................................... 377
Figure 43.12-14 SiC-100: Optical Assembly of NIRSpec for James Webb Space
Telescope .......................................................................................................... 377

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Figure 43.15-1 - Glass ceramics: Coefficient of thermal expansion with temperature materials for optical instruments in space.......................................................... 387
Figure 43.15-2 - Zerodur: Production process schematic.................................................. 388
Figure 43.15-3 - Zerodur: Annealing process .................................................................... 389
Figure 43.15-4 - Zerodur: Summary of engineering data .................................................. 390
Figure 43.15-5 - Zerodur: Optical transmission curve ....................................................... 391
Figure 43.15-6 - Zerodur: Thermal expansion cryogenic behaviour............................... 392
Figure 43.15-7 - Zerodur: Coefficient of thermal expansion different glass
ceramics ............................................................................................................ 392
Figure 43.15-8 - Zerodur: Thermal expansion of different glass ceramics ........................ 393
Figure 43.15-9 - Zerodur: Thermal conductivity characteristics of different glasses ......... 393
Figure 43.15-10 - Zerodur: Failure probability for test surfaces processed with
bonded grit of different sizes.............................................................................. 398
Figure 43.15-11 - Zerodur: Failure probability of Zerodur for test surfaces processed
with loose grit of different sizes.......................................................................... 398
Figure 43.15-12 - Zerodur: Failure probability, F, as a function of test surface area,
SL ...................................................................................................................... 399
Figure 43.15-13 - Zerodur: Bending strength under constant load.................................... 399
Figure 43.15-14 - ULE: Transmission curve ...................................................................... 403
Figure 43.15-15 - ULE: Thermal expansion characteristics............................................... 404
Figure 43.17-1 Technical ceramics: CVD diamond sand erosion .................................. 412
Figure 43.18-1 NIRSpec optical bench development: Cesic ceramic demonstrator
structure............................................................................................................. 416
Figure 43.18-2 NIRSpec optical bench development: Test set-up and I-beam
sample with joint line.......................................................................................... 417
Figure 43.18-3 NIRSpec optical bench development: Test set-up for instrumented
bench cells......................................................................................................... 417
Figure 43.18-4 NIRSpec optical bench development: Test set-up for shaker
vibration tests..................................................................................................... 418
Figure 43.18-5 NIRSpec optical bench development: Test set-up for cryogenic
temperature test................................................................................................. 418
Figure 43.18-6 NIRSpec optical bench development: Thermal contraction under
cryogenic test..................................................................................................... 420
Figure 43.18-7 NIRSpec optical bench development: Linear displacement under
cryogenic test..................................................................................................... 421
Figure 43.18-8 NIRSpec optical bench development: Out-of-plane displacement
under cryogenic test .......................................................................................... 421
Figure 43.19-1 Zerodur: Optical bench for LISA pathfinder mission................................ 423
Figure 44.5-1 - Magnesium alloys: Momentum wheel bracket for satellite - Example ......... 452
Figure 44.5-2 - Carbon fibre-reinforced magnesium alloy: Space mirrors
(experimental) - Example................................................................................... 453

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Figure 45.3-1 - Copper ODS alloys: Elevated temperature stress-rupture properties of
Glidcop ODS alloys compared with some high conductivity copper alloys........ 458

Tables
Table 34.8-1 - Detection of manufacturing defects by contact NDT techniques .................... 60
Table 34.8-2 - Detection of manufacturing defects by non-contact NDT techniques ............. 61
Table 34.8-3 - Detection of in-service damage by contact NDT techniques .......................... 62
Table 34.8-4 - Detection of in-service damage by non-contact NDT techniques ................... 63
Table 34.14-1 - Defect detection by shearography ................................................................ 87
Table 34.15-1 - Thermography: Summary of diameter/depth ratios from different
studies ................................................................................................................. 93
Table 34.15-2 - Thermography: Detection levels established for flat bottomed holes
(FBH) from ESTEC study .................................................................................... 93
Table 34.18-1 - Detection of damage by eddy current and ultrasonics................................ 103
Table 34.21-1 - Summary of NDT techniques for polymer composite space structures ...... 109
Table 34.23-1 - Interrelationship of items influencing the test.............................................. 112
Table 34.23-2 - Effects of local failure modes on global behaviour of the structure............. 113
Table 34.23-3 - Detection of techniques to various failures occurring during test................ 114
Table 34.23-4 - Interrelation between failure modes and their possible locations ............... 115
Table 34.23-5 - Interrelation between type of loading and possible failure modes .............. 116
Table 34.23-6 - Failure modes which have to be covered by the specific tests ................... 117
Table 34.23-7 - Appropriate instrumentation of particular areas of the structure ................. 118
Table 34.23-8 - Interrelation between particular areas of the structures and possible
dangerous loads ................................................................................................ 119
Table 34.23-9 - Testing of particular areas of the structure ................................................. 120
Table 34.23-10 - Load combinations for the relevant cases ................................................ 121
Table 34.23-11 - Testing different load cases ...................................................................... 122
Table 36.3-1 - Resin procurement: General Information...................................................... 143
Table 36.3-2 - Resin procurement: Base resin..................................................................... 144
Table 36.3-3 - Resin procurement: Hardener....................................................................... 144
Table 36.3-4 - Resin procurement: Catalyst......................................................................... 145
Table 36.3-5 - Resin procurement: Modifier......................................................................... 145
Table 36.3-6 - Resin procurement: Solvent.......................................................................... 145
Table 36.3-7 - Resin procurement: Blend ............................................................................ 146
Table 37.5-1 - Test data for HM carbon/epoxy specimen .................................................... 156
Table 38.3-1 - Wet lay-up and laminating: Troubleshooting guide....................................... 165
Table 38.3-2 - Hand wet lay-up: Selection factors ............................................................... 166
Table 38.3-3 - Process steps for prepreg lay-up .................................................................. 168

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Table 38.4-1 - Tooling for composites: Relative merits of various types for CFRP .............. 177
Table 38.12-1 EB curing: Advantages and drawbacks of epoxy and acrylate resins........ 195
Table 38.12-2 EB curing: Mechanical properties of some acrylate and epoxy resins....... 196
Table 38.12-3 EB curing: Typical mechanical properties of unidirectional IM carbon
fibre/acrylate resin ............................................................................................. 196
Table 40.3-1 - Cost optimisation: Eurostar Bus/Inmarsat 2 study ........................................ 241
Table 40.6-1 - Launcher fairing constructions: Mass and cost of various designs ............... 247
Table 40.6-2 - Launcher fairings: Kepner-Tregoe trade study evaluation criteria ................ 249
Table 40.7-1 - Selected thermoplastic component: Cost/producibility trade-off
analysis.............................................................................................................. 256
Table 40.7-2 - Selected thermoplastic components: Relative manufacturing costs and
major contributors to cost .................................................................................. 258
Table 42.6-1 - Reinforcing fibres available for use in inorganic composites ........................ 289
Table 42.6-2 - Continuous fibre and filament reinforcements used in MMCs and
CMCs................................................................................................................. 291
Table 43.2-1 Technical ceramics: Oxides - general features ............................................ 308
Table 43.2-2 Technical ceramics: Carbides - general features......................................... 309
Table 43.2-3 Technical ceramics: Nitrides - general features ........................................... 310
Table 43.2-4 Technical ceramics: Carbons - general features.......................................... 312
Table 43.2-5 Technical ceramics: Sources - examples..................................................... 314
Table 43.3-1 Technical ceramics: ISO standards - summary ........................................... 318
Table 43.3-2 Technical ceramics: ISO standards - drafts ................................................. 319
Table 43.4-1 Technical ceramics: green shape processes ............................................. 321
Table 43.5-1 Technical ceramics: Materials - mechanical components............................ 328
Table 43.5-2 Technical ceramics: Materials - thermomechanical components................. 329
Table 43.5-3 Technical ceramics: Materials - electrical .................................................... 330
Table 43.5-4 Technical ceramics: Materials optical and dimensionally-stable
structures ........................................................................................................... 331
Table 43.6-1 Technical ceramics: alumina typical properties......................................... 334
Table 43.6-2 Technical ceramics: ZTA zirconia toughened alumina typical
properties........................................................................................................... 335
Table 43.7-1 Technical ceramics: Aluminium nitride typical properties.......................... 337
Table 43.8-1 Technical ceramics: boron carbide typical properties ............................... 339
Table 43.9-1 Technical ceramics: boron nitride typical properties ................................. 343
Table 43.10-1 Technical ceramics: carbon types typical properties............................... 347
Table 43.10-2 Technical ceramics: carbon-graphite grades typical properties .............. 348
Table 43.10-3 Technical ceramics: carbon foams typical properties ............................. 350
Table 43.11-1 Technical ceramics: silica typical properties ........................................... 352
Table 43.12-1 Technical ceramics: silicon carbides comparison of materials
properties produced by different process routes ............................................... 355
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Table 43.12-2 Cesic: Mechanical properties .................................................................. 360
Table 43.12-3 Cesic: Thermal properties ....................................................................... 361
Table 43.12-4 SiC 54S: Mechanical properties ............................................................... 364
Table 43.12-5 SiC 54S: Thermal properties .................................................................... 365
Table 43.12-6 SiC 100: Manufacturing size constraints - practical size limitations
for finished part .................................................................................................. 370
Table 43.12-7 SiC 100: Typical characteristics ............................................................... 371
Table 43.12-8 SiC 100: Micro-VCM test E544 - outgassing values................................. 371
Table 43.13-1 Technical ceramics: silicon nitrides comparison of materials
properties produced by different process routes ............................................... 379
Table 43.14-1 Technical ceramics: partially stabilised zirconia typical properties ......... 381
Table 43.15-1 Technical ceramics: Zerodur glass typical properties............................ 384
Table 43.15-2 Technical ceramics: ULE glass typical properties ................................. 385
Table 43.15-3 - Zerodur: Characteristic strength, Weibull factor and stress corrosion
factor.................................................................................................................. 397
Table 43.15-4 - Zerodur: Fracture toughness of some glasses......................................... 400
Table 43.15-5 - ULE: Summary of engineering data ......................................................... 402
Table 43.17-1 Technical ceramics: CVD diamond typical properties............................. 409
Table 43.17-2 Technical ceramics: CVD diamond Weibull modulus.............................. 409
Table 43.17-3 Technical ceramics: CVD diamond Youngs modulus ............................ 410
Table 43.17-4 Technical ceramics: CVD diamond typical optical properties for
high-power laser systems .................................................................................. 413
Table 43.17-5 Technical ceramics: CVD diamond typical dielectric properties for
high-power microwave systems......................................................................... 414
Table 43.19-1 Zerodur: Overview of terrestrial astronomical telescope mirrors .............. 423
Table 44.1-1 - Magnesium alloys: ASTM designation system - alloys and tempers ............ 434
Table 44.1-2 - Magnesium alloys: Sources - examples ....................................................... 436
Table 44.2-1 - Magnesium alloys: Nominal chemical compositions..................................... 438
Table 44.2-2 - Magnesium alloys: Typical mechanical properties, at room
temperature ....................................................................................................... 440
Table 44.2-3 - Magnesium alloys: Typical low temperature tensile properties at 196C................................................................................................................. 442
Table 44.2-4 - Magnesium alloys: Typical tensile properties at elevated temperatures....... 443
Table 44.2-5 - Magnesium alloys: Typical elevated temperature creep properties .............. 444
Table 44.2-6 - Magnesium alloys: Typical fatigue and fracture toughness properties at
room temperature .............................................................................................. 445
Table 44.2-7 - Magnesium alloys: Damping capacity of selected alloys and other
metals ................................................................................................................ 446
Table 44.3-1 - SiC particulate reinforced AZ61 magnesium alloy: Typical mechanical
properties........................................................................................................... 447

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Table 44.3-2 - SiC particulate reinforced magnesium alloy: Typical mechanical
properties........................................................................................................... 448
Table 44.4-1 - Continuous fibre reinforced magnesium MMC materials: Examples ........... 448
Table 44.4-2 - Magnesium continuous reinforced MMCs: Typical mechanical
properties........................................................................................................... 450
Table 45.3-1 - Copper ODS alloys: Ambient temperature tensile properties ....................... 459
Table 45.3-2 - Copper ODS alloys: Short term properties at 538C .................................... 460
Table 45.3-3 - Copper ODS alloys: Creep strength at 538C .............................................. 460
Table 45.5-1 - Continuous fibre reinforced copper: Thermal conductivity of carbon/Cu
and carbon/Al composites ................................................................................. 462

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Introduction
TheStructuralmaterialshandbook,ECSSEHB3220,ispublishedin8Parts.
Aglossaryofterms,definitionsandabbreviatedtermsforthesehandbooksiscontainedinPart8.

Thepartsareasfollows:
Part1

Overviewandmaterialpropertiesandapplications

Clauses19

Part2

Designcalculationmethodsandgeneraldesignaspects

Clauses1022

Part3

Loadtransferanddesignofjointsanddesignofstructures

Clauses2332

Part4

Integritycontrol,verificationguidelinesandmanufacturing

Clauses3345

Part5

Newadvancedmaterials,advancedmetallicmaterials,
generaldesignaspectsandloadtransferanddesignofjoints

Clauses4663

Part6

Fractureandmaterialmodelling,casestudiesanddesignand
integritycontrolandinspection

Clauses6481

Part7

Thermalandenvironmentalintegrity,manufacturingaspects, Clauses82107
inorbitandhealthmonitoring,softmaterials,hybrid
materialsandnanotechnoligies

Part8

Glossary

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33
Aspects of damage tolerance
33.1

Introduction

33.1.1

Damage tolerance

Damagetoleranceistheabilityofacompositematerialstructuretoresisttheonsetofdamageand
perform to the stipulated design parameters, with damage present, throughout its remaining life
time.
TheguidelinespresentedaretobereadinconjunctionwithnormativeECSSstandardsECSSQST
20;ECSSQST40;ECSSQST70;ECSSEST30seriesandECSSEST3201.

33.1.2

Damage events

Composite structuresareusually exposed toa variety ofevents during their life. This can include
normal inservice loading, inservice events that result in damage initiation and structural
degradation,alongwithenvironmentrelatedevents.
Damagecanalsooccurduringmanufactureorhandlingbeforethestructureentersservice.
The ability of a composite material to resist certain potential damage events is known as damage
resistance.Itdiffersfromdurabilitybecausedurabilityaddressesthepreventionofdamageunder
normaloperatingconditions.

33.1.3

Damage tolerance criteria

Many agencies impose damage tolerance criteria. The details of such criteria are tailored to the
structureofinterest,althoughtherearesomecommonthemes,[See:33.3]:

Defectsareoftenstandardisedforanalysispurposes,[See:33.4],i.e.

defectsthatcanariseduringmanufacture,[See:19.2],

damagethatcanoccurwhilstinservice,[See:19.3].

The effect of macroscopic defects on static load; failure modes and the use of fracture
mechanics,[See:33.5].

Testing and analysis: cyclic loading, nogrowth criterion, residual strength and inspection,
[See:33.6].

Environmentrelated aspects, e.g. flammability, lightning and other protection systems,


acousticfatigue,impactdynamics,[See:33.7].

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33.2

General guidelines

33.2.1

Fracture control

Thedamagetoleranceevaluationoflaminatedcompositestructuresisbasedonthefracturecontrol
requirements of normative standard ECSSEST3201, [See also: 34.10 for analysis and test
documentation]

33.2.2

Durability

Durability considerations are typically combined with damage tolerance to meet economic and
functionality objectives. Specifically, durability is the ability of a structural application to retain
adequateproperties,e.g.strength,stiffness,andenvironmentalresistance,throughoutitslifetothe
extent that any deterioration can be controlled and repaired, if there is a need, by economically
acceptablemaintenancepractices,Ref.[332].
Durability largely addresses economic issues, while damage tolerance is focussed on safety. For
example,durabilityoftenaddressestheonsetofdamagefromtheoperationalenvironment.Under
the principles of damage tolerance design, the small damages associated with initiation can be
difficulttodetect,butdonotthreatenstructuralintegrity,Ref.[332].

33.2.3

Damage

The location of damage initiation sites are often difficult to identify and thorough inspections are
neededusingtraditionaltechniquesandNDTnondestructivetestingtechniques.
Inmanymetals,failureinvolvesthegrowthofasmallcrackperpendiculartotheappliedstress.
By contrast, in laminated composite materials stress relaxation and fracture results from
combinationsof:

Splittingparalleltothefibres,

Matrixmicrocracking,

Fibrefailure,

Delamination,

Pullingoutoffibres,

Pullingoutofcompleteplies.

33.2.4

Defects in composites

33.2.4.1

General

Defectsincompositeelementscanbedescribedaseither:

Globaldeviations,or

Localimperfections.

Figure33.2.1summarisesthevarioustypesofdefectsthatcanoccurincompositematerials,Ref.[33
4].

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33.2.4.2

Global

Globaldeviationsarerelatedto:

Acompleteelement,or

Alargeareaofanitem.

The effect of a global deviation is to reduce the capability of an element. The level of reduced
performance is dependent on the particular deviation, e.g. that occurring within a cure cycle.
Adequatecontrolcanbeachievedby,[Seealso:Chapter19]:

Aprocesscompanionsample;alsoknownasawitness,or

Nondestructivechecksofkeypoints.

As the whole item is affected, control is related more to the quality, i.e. coverage of all potential
sourcesofdegradation,thantoquantity.

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Macroscopic ply defects


Wrinkles, waviness, misalignment
Prepreg variability exceeds pre-set values
Local resin enrichment
Fibre starved areas
Porosity, voids
Contamination
Variable cure, oven temperature inhomogeneity
Non-uniform agglomerations of hardener
agents
Laminate defects
Interlaminar defects by delamination:
- at edges and corners (splintering)
- inside (blister)
Resin enrichment:
- interlaminar
- on outer surface
Surface defects:
- scratches with fibre breakage
- dents without fibre breakage
- fibre break away from impact
Foreign particles
Ply incorrect:
- missed
- wrong material
- missed orientation
- overlap
- underlap gap
Cracks at edges or corners

Component defects
Holes:
- oversized holes
- breakout or broken fibres on hole exit
- mislocated and repaired holes (resin)
- out-of-round hole
- resin-starved bearing surfaces
Fasteners
- tear-out or pull-through in countersink
- over-torqued or undersized fasteners
- improper seating of fasteners
- tool impressions
Thickness deviation on:
- manufactured hardware
- process control coupons
Non-uniform bond thickness
Warpage on:
- detailed parts
- assembled parts

Figure33.21Summary:Defectsincompositematerials

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33.2.4.3

Local

Local imperfections, identified by microscopic inspection of composite materials, identifies local


irregularities,suchas:

Nonuniformdistributionofresinandfibres.

Interruptedorbrokenfibres.

Disbondsatfibretomatrixinterfaces.

Voids.

Inclusions.

Astheselocaldefectsarestatisticallydistributed,theyarecoveredbythelowerboundofmaterial
properties.
Significantlylarger imperfections can cause progressive failure.Only local macroscopic deviations
areconsideredhere,whichalthoughmacroscopic,thevolumeofacriticallocaldefectcanberather
small.Adequatecontrolprocedurespreventsuchpotentialdefectsoccurringinthewholeitem.
The screening of the structure needs to be performed with sufficiently highresolution, sensitivity
andreliability.Thereforethecontrolproblemsrelatetobothqualityandquantity.

33.2.4.4

Proof test

The use of proof testing for flight articles, as a means of damage tolerance demonstration, can be
consideredonacasebycasebasis.Inconsideringanysuchdemonstration,itisnecessarytoreview
thetestlevelandensurethat:

Thetestdoesnotintroduceanyunwarranteddamage,and

Theworstlimitloadcasesarecoveredbysuchatest.

33.2.5

Impact damage

33.2.5.1

Laminates

Impactdamageiscontainedwithinthelaminateitself.

33.2.5.2

Sandwich structures

Incontrasttolaminates,insandwichconstructionstherearetwoloadpathsseparatedbyacorethat
isresponsibleforshearloadtransfer.

Impactdamageistypicallyunsymmetrical,sothisneedsabetterunderstandingoftheprogression
ofthedamageandtheresidualstrength.Damagetoleranceofsandwichstructuresismorecomplex
thanlaminatedstructuresasdamagecaninclude:

Penetrationordelaminationofthefacings;sometimesboth.

Corecrushing

Facingtocoredebonding

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Cores tend to absorb and retain moisture which can reduce mechanical properties as well as
increasingthestructuralweight.
Typicallyimpactdamageisnotuniformthroughthethicknessofthesandwichstructure,sincean
impactor or projectile can penetrate or damage the outward facing skin whilst the inner skin
remainsundamaged.
Compositefacingsorskinsonsandwichstructurestypicallyfailasaresultof:

Matrixcracks

Fibrefracture

Fibrebuckling

Delamination.

Ifonlyonefacingisdamagedsignificantly,thiscancausearedistributionofstressesinthedamaged
facesheet.
Visualinspectionsfordamagethenbecomemoredifficultbecausethecorecanmaskthedamageor
hindertheeffectivenessofanondestructiveevaluationtechnique.

33.3

Damage tolerance criteria

33.3.1

General

33.3.1.1

Types of flaw

Forcompositestructuresthedamagetolerancephilosophyisprimarilyconcernedwiththetypesof
flaw,i.e.:

Alargeundetectedmanufacturingdefect,whichcanbeassumedtobeaninclusionorother
defectthatcausesadelamination.

A surface scratch, where the length and depth of the scratch is defined and the orientation
andlocationisassumedtobeinthemostcriticallocationforagivenstructure.

Undetected impact damage, where the damage area is assumed to be consistent with BVID
barelyvisibleimpactdamageandinacriticallocation,[Seealso:19.5].

Anundetectedimpactdamageisthemostseriousofthetypesofflawformanystructures.

33.3.1.2

Effect of flaw

Incompositestructures,assumptionsaremadeabouttheflaws,i.e.:

Thegrowthofaflawisunstable.

Theinitialflawdoessignificantlyaffectthestaticstrength.

Themainaimistoreducemaintenancebytheuseofanalysisandtestingtodemonstratethat
thedamagedoesnotamounttoasafetyriskoverthedesignlifeofthestructure.

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33.3.1.3

Threats

To construct a damage tolerance assessment for composite structures, the threats are defined for
eachstructure,.i.e.:

Damagefrommanufacturingprocesses.

Accidentaldamagefromassemblyandhandling.

Accidentaldamagefrominserviceoperation.

33.3.1.4

Modes of damage

The next step is to define the modes of damage for each threat, e.g. porosity, delamination,
puncture,crushedcore.
Foreachmodeofdamage,characteristicssuchasinitialflawsize,thresholdofdetectability,critical
size,andwhethergrowthduringloadingaredefined.
In many composite structures subjected to spectrum or block cycle loading, the growth of impact
damageischaracterisedbyperiodsoflittleornogrowthatalowloadlevelfollowedbyrelatively
large growth at relatively high loads. A significant effect of impact damage is the significant
reduction in static strength once the impact has occurred and often the most critical damage is
inducedbyalowvelocityimpactevent,[Seealso:19.5].
Themostcriticalmodeofloadingformetallicstructureistension,whichcausescrackopening.The
critical modes of loading for composite structure is identified for purposes of selecting principal
structuralelementsandfordevelopingappropriatetesting.

33.3.2

Load paths

Indamagetoleranceassessments,anogrowthcriterionisappliedindemonstratingtheintegrityof
individualloadpathsortheindependenceofloadpaths.

33.3.3

Environment

Structuraldetails,elements,andsubcomponentsofcriticalstructuralareas,designatedFCIsfracture
criticalitems,aretestedunderenvironmentalloadsrepresentativeofoperationalusage.Thistesting
canformthebasisforvalidatinganogrowthapproachtothedamagetolerancerequirements.The
testingassessestheeffectoftheenvironmentontheflawgrowthcharacteristicsandthenogrowth
validation.

33.3.4

Damage

Damage levels, including lowlevel impact damage, typical of those that can occur during
fabrication,assemblyandoperationareintroduced.Theextentofsuchinitiallydetectabledamageis
establishedand is consistent with the inspection techniques employed duringmanufacture and in
operation.
Flawordamagegrowthdataisobtainedfromoperationrelatedloadcyclingofsuchintrinsicflaws
ordelaminationsormechanicallyintroduceddamage.
Thenumberofcyclesneededtovalidateanogrowthconceptisstatisticallysignificantandcanbe
determinedbysuchloadorlifeconsiderationsasreflecttheoperationalusage.Thegrowthorno

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growthevaluationisestablishedbytestssupportedbyanalysisorbytestsatthecoupon,elementor
subcomponentlevel.
Anogrowthevaluationisapplied,unlessthereissufficientevidenceforgrowthevaluation.Thisis
relatedtotheoperationaluseinspectionprogrammebeingacceptablefortheparticularFCI.

33.3.5

Residual strength

The extent of damage for the residualstrength assessments is established. Residualstrength


evaluation by component or subcomponent testing or by analysis supported by test evidence is
performedconsideringtheparticulardamage.

33.3.6

Safe-life

In the case of a safelife demonstration, the evaluation demonstrates compliance with the fracture
controlrequirementsofECSSEST3201.

33.3.7

Fail-safe

In the case of failsafe structures, the residual strength is sufficient to permit the safe operation at
limitloadsthroughoutthetimeintervalbetweenscheduleinspections.

33.3.8

Stiffness

It is also demonstrated that the stiffness properties have not changed beyond acceptable levels in
relationtoaeroelasticandanyotherstiffnessrequirementsasaresultofthedamageidentifiedfor
theresidualstrengthassessments.

33.3.9

Loads

Thestructureisabletowithstandstaticloads,consideredaslimitloads,thatareexpectedduringthe
completionoftheservicelifeonwhichdamageresultingfromobviousdiscretesourcesoccur,e.g.
dropped tools, meteoroid impact. The extent of damage is based on each discrete source. This
damagedefinitionandanyverificationprogrammeisthesubjectofreview.

33.3.10 Environmental factors


Theeffectsoftemperature,humidityandotherenvironmentalfactorswhichcanresultinmaterial
propertydegradationareaddressedinthedamagetoleranceevaluation.

33.3.11 Inspection
An inspection programme is developed consistingof frequency, extent andmethods of inspection
forinclusioninthemaintenanceplan.
Theinspectionintervalsareestablishedsuchthattheextentofthedamageiscarefullycheckedwith
respect to the residualstrength capability including the nogrowth design concept. Any areas
deemednoninspectablearesubjectofaspecialdesignandtestprogramme.

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33.3.12 Summary
Themainstagesofadamagetoleranceevaluationare,Ref.[331]:

Selecttheprincipalstructuralelementstobeevaluated.

Defineordevelopforeachlocation:

stressspectrum.

environment.

crackgrowthratedata.

fracturetoughnessdata.

structuralcategory.

criticaldamagesizeunderlimitloadandinserviceload.

crackgrowthcurvesfromspectrumloading.

Establishinitialdamagesize.

Establishdamagethresholdofdetectabilityforeachlocation.

Validateresidualstrengthandcrackgrowthanalysismethodswithtesting.

33.4

Defect standardisation

33.4.1

General

33.4.1.1

Metal structures

Theassessmentofdefectsinhomogeneousandisotropicmetallicstructuresbyfracturemechanics
stillinvolvessimplifications.Therealvolumetricdefect,e.g.apore,isconservativelyrepresentedby
a mathematical cut of the size of its projection; as shown in Figure 33.4.1. The sharp edges of the
assumedcrackaremoreseverethanthoseofrealdefects.

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Figure33.41Metalstructures:Idealisationofavolumetricdefect
33.4.1.2

Composite structures

Theassessmentoftheeffectofdefectsneedsasimplifiedrepresentationoftherealdefectinorderto
reducethecomplexityaddedbythematerialheterogeneityandanisotropy.
Likefracturemechanics,afewstandardtypesofdefectscovermostlocaldeviations.Thisappliesto:

Assessmentandverification,and

Degreeofresolutioninnondestructiveinspection

33.4.2

Types of defects

Forthesimplificationofrealdefects,[See:Chapter19],thefactorstoconsiderinclude:

Localdefects:Forthethinlaminatesoftenusedforlightweightspacestructures,mostlocal
defects can be represented by a throughthethickness defect. It is difficult to justify that a
surface defect, e.g. a severe scratch in a laminate having a few plies, relates to a part of the
pliesonly,sothisapproachisnotconsideredtobetooconservative.

Delaminations: The separation of plies can be a source of primary failure in a composite


structure under compressive loads. Very local delaminations in the vicinity of notches are
knowntoreducetheeffectofthestressconcentrations.

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Circular defects: Experience shows that circular defects, through a laminate, usually have a
slightly higher influence on residual strength than slots having a length equivalent to the
diameter.

Standardiseddefectsthatenableanassessmentofmosttypesofmanufacturingandoperationally
induceddefectsare:

Circularholes,and

Circulardelaminations.

Figure33.4.2showstheidealisationofrealdefectsincompositestructuresusingastandardcircular
defect.

Figure33.42Compositestructures:Idealisationofdefectsbystandardcircular
defect

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33.5

Effect of macroscopic defects on static load

33.5.1

Composite failure

Incompositematerials,mainlyCFRP,fracturebehaviourisprimarilyelastic,i.e.thereisnoplastic
deformationcomparedwiththatofductilemetals.
Materials with such brittle failures are sensitive to notches and cracks under static and cycling
loading,especiallywithrespecttoresidualstrengthunderquasistaticloads.
Careful observation of the failure process during testing of notched specimens shows that under
steadily increasing loads, the failure initiates within individual plies, either along or transverse to
fibres, but also between certain plies long before the maximum load capability is reached. The
partialdamagewithinorbetweencertainpliesproducesaredistributionofthelocalstressesthatin
turnresultsinacomplicated,interactivefailureprocess.
Anyattempttorelatethefinalfailuretothedistributionofinitialstressesisquestionable.

[Seealso:Chapter14]

33.5.2

Use of fracture mechanics

33.5.2.1

Isotropic materials

ThewideapplicationofLEFMlinearelasticfracturemechanicstohomogeneousisotropicmaterialis
supportedbyitsrelativesimplicity.Oneparameter,thetoughness,candescribethefailureloadofa
precrackedelement.

33.5.2.2

Anisotropic plates

Theconditionsunderwhichthetechniquesofisotropicfracturemechanicscanbedirectlyappliedto
anisotropicplatesaredescribed.

33.5.3

Multi-angle laminates

The conditions cannot be maintained correctly for multiangle laminates. The inhomogeneity is
createdbythe:

Fibre/matrix(microheterogeneity),and

Stacking(macroheterogeneity).

Withtheintenttogenerateafailurecriterionphenomenologically,onecanconsiderthelaminateto
besufficientlyhomogeneousforthestressesresultingfromexternalloadingtoberelatedtothetotal
thicknessofthelaminate(grossstresses).
Implicitly, with the assumption of homogeneity, the considerations are limited to defects passing
throughthethickness,i.e.holes.
Furthermore, as the toughness of unidirectional laminates is different under longitudinal and
transverse loading, the toughness of an arbitrary multiangle laminate cannot be expected to be a
materialconstant.

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Inphenomenologicalfracturemodels,theinitiationandpropagationofdamage,occurringwithinor
betweenthedifferentplies,longbeforethecriticalloadingisreachedarerecognisedbyassumingan
effectivesizeofdefectwhichislargerthanthegeometricdimensionsofthenotch.

33.6

Test and analysis

33.6.1

General

33.6.1.1

Scope

The nature and extent of analysis or tests on complete structures, or portions of the primary
structure, depend upon applicable previous damagetolerant designs, construction, tests and
operational experience on similar structures. In the absence of experience with similar designs,
approvedstructuraldevelopmenttestsofcomponents,subcomponentsandelementsareperformed.

33.6.1.2

Location

Since there are a large number of locations on each composite structure to be evaluated, it is
impractical to evaluate the damage tolerance at each location by testing. Analysis is therefore
needed.Theanalysisproceduresassociatedwithdamagetoleranceevaluationarebasedonfracture
mechanics,whichincludestressintensity,interlaminarfracturetoughnessandpropagationgrowth
ratesofcracksordelamination.

33.6.1.3

Strength

Analytical calculations are used for residual strength calculations and fatigue analyses under
spectrum loading, which are two major ingredients in damage tolerance evaluation. Sufficient
testingisneededtovalidatetheanalysismethods.Fullscalestructuraltestingoccurstoolatetobe
usefulduringthedesignphase,butitisusedlatertoenableinitialdamagetoleranceevaluationsto
beupdated.

33.6.1.4

Environment

The effects of environment can be accounted for in both the analysis stage of the assessment and
duringthematerialscharacterisationstage.
The effects of moisture diffusion and temperature can be included as an additional loading
conditionintheanalyses.Additionally,theeffectsofmoistureandtemperatureonthedelamination
characterisationpropertiescanbedeterminedbyconductingtestsunderhostileconditionsorafter
ageing(longtermoraccelerated)ofthematerialsconsistentwiththeirapplication.

33.6.1.5

Tests

Aspartofthedamagetoleranceapproach,testsareclearlydefinedandperformed,Ref.[332]:

static testing of structural elements with various modes of damage and various modes of
loadingtoprovideresidualstrengthinformation

cyclic testing of structural elements with various modes of damage and various modes of
loadingtoprovidedamagegrowth(ornogrowth)information

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Cyclictestingofimportantfullscalecomponentstoverifythatdamagewouldnotgrowtoa
criticalsizeinthefullscalearticleduringthelifeofthestructure

Static testing of important fullscale components to verify that they would carry required
loadswithanydamagegrowthinflictedfromcyclicloading

Appropriatetestingtovalidateanyanalysesmethodsused

33.6.1.6

Test programme

Theapproachtakenforcompilingatestprogrammefrommaterialsselectiontostructuralvalidation
isknownasthebuildingblockapproach;asshowninFigure33.06.1,[Seealso:33.2].
Theadvantageoftheapproachisthatitenables:

Identification by experimentation of the multiplicity of failure modes that composite


structurescanexperience.

Identification of knockdown or enhancement factors for environmental conditions, when


testingoffullscalestructuresinahostileenvironmentisnotfeasible.

Theapplicationofrealisticserviceloadsandenvironmentsto thetestcouponorsubstructureare
emphasisedwithinthisapproach.

Crippling

Figure33.61Buildingblockapproach:Testprogrammedevelopment

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33.6.1.7

Composites

Fivelevelsoftestsarenecessaryforcomposites;asshowninFigure33.6.2:

Constituent,

Lamina,

Laminate,

Structuralelement,

Structuralsubcomponent.

Figure33.62Buildingblockapproach:Compositematerials

33.6.2

Constituent tests

The individual properties of fibres, fibre forms, matrix materials, and fibrematrix preforms are
evaluated.Thekeypropertiesinclude:

Matrixdensity,

Fibredensity,

Fibretensilestrength,

Fibretensilemodulus.

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33.6.3

Lamina tests

The properties of the fibre and matrix together in the composite material form are evaluated. The
keypropertiesinclude:

Fibrearealweight,

Matrixcontent,

Voidcontent,

Curedplythickness,

Laminatensilestrengthsandmoduli,

Laminacompressivestrengthsandmoduli,

Laminashearstrengthsandmoduli.

33.6.4

Laminate tests

Laminate testing characterises the response of the composite material in a particular laminate
design,suchasquasiisotropic.Thekeypropertiesinclude:

Tensilestrengthsandmoduli,

Compressivestrengthsandmoduli,

Shearstrengthsandmoduli,

Interlaminarfracturetoughness,

Fatigueresistance.

33.6.5

Structural element and component tests

The ability of the material to tolerate common laminate discontinuities is evaluated. The key
propertiesinclude:

Openandfilledholetensilestrengths,

Openandfilledholecompressivestrengths,

Compressionafterimpactstrength,

Jointbearingandbearingbypassstrengths.

33.6.6

Structural sub-component or full-scale tests

Thebehaviourandfailuremodeofincreasinglymorecomplexstructuralassembliesareevaluated.
Theselectionofwhichisstructureandapplicationdependent.

33.6.7

Delamination

33.6.7.1

In-service

Thethreatofdelaminationarisingfrominserviceloadinghasbeenoneofthefactorsinlimitingthe
adoptionoflaminatedcompositematerialsingreatervolumeforprimarystructure.

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While other damage modes such as matrix cracks can occur first, delaminations result in larger
stiffnessdropsandreductioninloadbearingcapabilities.
Delaminations can occur from interlaminar stresses arising from geometric or material
discontinuities from design features, e.g. an edge, a hole, a dropped ply. However, they can also
occur from matrix cracks or from interlaminar stresses caused by structural loading, such as in a
curvedlaminate,orbyforeignbodyimpacts.
A delamination, once initiated, grows under fatigue loads. During delamination growth, the
structuralloadscanberedistributedsuchthatanotherdelaminationoccursinanotherlocation.
The delaminations can continue to grow and accumulate until a structural failure occurs, such as
bucklingorfibrefailure.
Alternatively,thedelaminationcanbearrestedandthestructuremaintainssomelevelofintegrity.
Although delamination does not always cause a total loss of the loadbearing properties of the
component, it is usually a precursor to such an event. Therefore, knowledge of the resistance of a
composite to interlaminar fracture is useful not only for product development and material
screening, but a generic measurement of the interlaminar fracture toughness of the composite is
usefulforestablishingdesignallowablesfordamagetoleranceanalysesofcompositestructures.

33.6.7.2

Role of interlaminar fracture tests

Interlaminarfracturetestsareperformedbymanufacturingtestsampleswithprecracks.Thetypeof
testisdefinedbasedonthemodeofloadingofthetestsample,i.e.

ModeItestssuchasDCB

ModeIItestssuchas4ENF,ELS,ENF

ModeIIIECT,SCB(modified)

MixedModeI/IItestssuchasMMB,FPS/ADCB,CLS,stabilisedMMB

33.6.7.3

Dynamic loading

In most cases the components experience spectrum fatigue loads rather than constant amplitude
fatigue loads. For Mode I testing, the load needs to remain in tension. Therefore, the parts of the
spectrumwheretheloadcausesthedelaminationtoclosearerepresentedbyzeroloadintheDCB
tests.
With appropriate fixture design, the mode II test specimen can be loaded through zero and thus
fullyrepresentadelaminationinastructurewherethespectrumcontainstensionandcompressive
loads.
When the delamination has compressive loads closing the delamination (equivalent to a negative
GI),theinfluenceoffrictionandsubsequentheatingcanbeanissue.
Forafullcharacterisationforspectrumloads,thedelaminationonsetcurvesandthedelamination
growthcurvesaregeneratedfordifferentRratiosandblocksofloadingtoestablishthesynergistic
effects.

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33.7

Other features of damage-tolerance design

33.7.1

Acoustic fatigue

The resistance of the composite structure to noise damage is demonstrated by analysis or test. In
particular,itisdemonstratedthatnogrowthdamageareas,asestablishedinrelationtoquasistatic
loadingcriteria,donotpropagate.

33.7.2

Proof testing

Withinthefracturecontrolrequirements,allcompositestructuresandcomponentsareclassifiedas
potentiallyfracturecriticalitems,PFCI,[See:ECSSEST3201].

33.7.3

Metallic parts

Compositecomponentscancontainmetallicparts,e.g.attachmentfittingsorlargersubstructuresin
areasofhighloadtransfer.
Specialattentionispaidtofracturecriticalitems,FCIs.toinvestigatethetreatmentofareasofhigh
loadtransferinordertoensurethereisnounacceptablelocalyieldingwhendesignultimateloads
aresustained,[See:ECSSEST3201].

33.7.4

Thermal and meteoroid protection system

Theinterfacewiththecompositestructureandanythermalprotectionsystemistakenintoaccount
intheselectionofFCIs,andrelatedinspectionandmaintenance.
Any interactive effects in relation to local loadings, such as the response to impact loads and
acousticexcitation,arealsoconsidered.

33.7.5

Impact dynamics crashworthiness

Crashworthinessisdemonstratedbytestorbyanalysissupportedbyteststhat,underrealisticand
survivable conditions, the survival characteristics are commensurate with those achievable with a
conventionalmetallicaircraftstructure.

33.7.6

Flammability, toxicity and off-gassing

The properties of materials and processes used in space systems are established according to
normativeECSSstandards.

[See:ECSSQST70;ECSSQ7071]

[See also: ESMAT website for outgassing and flammability data from the ESTEC Materials and
Processesdatabases]

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33.7.7

Lightning protection

It is demonstrated by appropriateanalysis and testthat the structure can dissipate static electrical
charges,providenecessaryelectromagneticprotectionandprovideanacceptablemeansofdiverting
electricalcurrentarisingfromthelightningstrikesothatthevehicleisnotendangered.
A test and inspection procedure is established to ensure satisfactory maintenance of the lightning
protectionsystem.

33.8

Improving damage tolerance with higher


toughness laminates

33.8.1

General

Changes made to various composite material parameters can cause the notch sensitivity to range
frominsensitivetoverysensitive.Someguidelinesforcreatingtoughlaminatesarepresented,Ref.
[332].

33.8.2

Material-related aspects

33.8.2.1

Fibre-to-matrix bond

Toobtainatoughlaminate,thestrengthoftheinterfacialbondbetweenthefibreandmatrixhasto
beoptimised.Thisisachievedbycorrectsurfacetreatmentofthefibre.Ifthebondistoostrong,the
materialalwaysfailsinabrittlemannerirrespectiveoflayup.

33.8.2.2

Types of fibres

Materials which can store large amounts of strain energy are expected to be tough. Consequently
fibres with high strength, intermediate modulus and high failure strain are expected to be good
candidates for a tough laminate. Hybridisation provides much scope for developing composites
withincreasedtoughness.

33.8.2.3

Plies

Althoughtheinterlaminarfracturetoughnessofalaminatedoesnotappeartovarywithspecimen
thickness,ithasbeenshowntobesensitivetothethicknessofindividualplies.
In general, thick plies delaminate more easily and therefore decrease the interactions between
adjacentcrackedanduncrackedplies,soincreasingthetoughness.However,itisrecognisedthata
compromise can be made for other mechanical properties, such as fatigue and environmental
response.Itisgenerallywidelyrecognisedthatthickerpliesincreasethesusceptibilitytotransverse
crackingbyanincreaseinvolumeofmaterialunderstress.

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33.8.3

Lay-up aspects

33.8.3.1

Stacking sequence

Whiletheeffectsofstackingsequenceonthenotchedstrengthareunclear,ithasbeenshownthat
arranging plies to encourage delaminations between shear cracks in 45 plies and adjacent load
bearing0fibres,e.g.[45,0,0]s,resultsinahighernotchedstrength.
If,however,thedelaminationissuppressed,e.g.[0,45,0]s,thentheshearcracksthatdevelopin
the 45 plies at relatively low stresses have a detrimental effect on the 0 fibres. This results in a
relativelybrittlebehaviourwiththe0fibresfailinginastepwisemanneralongthe45line.
The [45]s layups, although they are relatively weak, are notch insensitive. Large damage zones
developacrosstheentirewidthofatestspecimenresultinginacontrolled,noncatastrophicfailure.
Owing to their relative weakness in the longitudinal directional, [45]slayups are unlikely to be
used to resist tensile loads alone. However, they can be used as crackarrest strips in a laminate
containingfibresintheloadbearingdirection.

33.8.3.2

Reinforcement style

The style of reinforcement has an important effect on the notched strength. In cases where the
formationofadamagezoneislargelysuppressed,arelativelybrittlebehaviouroccurs.Changesin
plyorientationarealsoknowntoaffectthenotchedstrength.

33.9

References

33.9.1

General
[331]

J.Tomblinetal
Reviewofdamagetoleranceforcompositesandwichairframe
structures
August1999

[332]

MILHDBK17:Polymermatrixcomposites

[333]

ESAPSS03207Guidelinesforcarbonandotheradvancedmaterial
prepregprocurementspecifications;nottransferredtotheECSS
documentsystem

[334]

MBB/ERNO
Integritycontrolofcarbonfibrereinforcedplastics(CFRP)structural
elementsExecutivesummary
ESAContract4442/80/NL/AK(SC)

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33.9.2

ECSS documents
[See:ECSSwebsite]
ECSSEST30series:
ECSSEST3208
ECSSEST3201
ECSSQST20
ECSSQST40
ECSSQST70
ECSSQ7071

33.9.3

Mechanical
Materials
Fracturecontrol;previouslyESAPSS
01401.
Qualityassurance
Safety
Materials,mechanicalpartsand
processes;previouslyESAPSS0170
Datafortheselectionofspace
materialsandprocesses;previously
ESAPSS01701

MIL standards

MILHDBK17

Polymermatrixcomposites

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34
Inspection and quality assurance
34.1

Introduction

An inspection programme is undertaken on components and assembled structures, carried out in


conjunction with defined quality assurance procedures. Detailed and explanatory documents are
keptonallaspectsofintegritycontrol.
Inspection using more than one nondestructive testing technique can be necessary. In addition,
NDTcanbecarriedoutinconjunctionwiththemechanicaltestingorproofloadingofcomponents
andassembledstructures.Forreusableandlonglifestructures,inserviceinspectionisalsodefined.
Points to be considered with respect to the philosophy of inspection and the application of
techniquesare:

Duringthedesignofstructures,considerationisgivenastohowtheassembliesareinspected
inordertodetectandcharacteriseanysignificantdefectsoranomalieswhichcanoccur.

It is preferable to enhance production quality procedures to minimise the occurrence of


manufacturingdefects,ratherthanrelylateroninspectiontocoveralleventualities.

Providedthatsufficientforethoughtisgiventodamagetolerantdesign,anexampleofanapproach
appliedisultrasonictestingatthepreassemblycomponentlevel,whichisthenfollowedbyvisual
inserviceinspection;aspartofpostqualificationoracceptancetesting.

34.2

Fabrication and quality assurance

34.2.1

Quality assurance

ECSSQST20 and the associated standards give details of the quality assurance system. These
requirementsaimtoguaranteethequalityandreproducibilityofthebasiccompositematerials.

34.2.1.1

Material procurement specification

Inestablishingaprocurementspecificationforcarbonandotheradvancedfibreprepreg,guidelines
areprovidedinRef.[3439].
Asaminimum,aprocurementspecificationcontains:

Basicfibreproperties,includingtype,numberandfrequencyoftest.

Basicmatrixpropertiesandchemicalcharacterisation,includingtype,numberandfrequency
oftest.

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Basiccompositeproperties,includingtype,numberandfrequencyoftest.

Condition of fabrication, including the process method, layup, tooling, workshop


environment.

Significantparametersofthecurecycle,e.g.time,temperature,pressure.

Curedcomponentproperties,includingtype,numberandfrequencyoftest.

Inspectioncriteria,ateverystage.

Storageandhandlingconditions,throughouttheprocesses.

Thestrictapplicationandcontrolofsuchspecificationsguaranteethequalityandreproducibilityof
theproduct.Nomodificationofthespecificationismadebeforeallofthesubsequenteffectsonthe
qualityofthestructurehavebeenverified.

34.2.1.2

Composites quality control plan

Aspecificqualitycontrolplanforthecompositethatensuresthenecessaryliaisonbetweendesign,
engineering,manufacturingandqualitydisciplinesisestablished.Thisplandefinestheproduction
routeandtheimportanceofanydefectslikelytooccurduringthefabricationprocess.Itisadaptable
to any special engineering requirements that arise with individual composites parts or areas as a
resultof:

Potentialfailuremodes,

Damagetoleranceandflawgrowthrequirements,

Loadings,

Inspectability,and

Localsensitivitiestomanufactureandassembly.

34.3

Inspection, maintenance and repair

34.3.1

Inspection and maintenance

34.3.1.1

General

Anondestructiveinspection(NDI)programmeisdevelopedthatdefinesthefrequency,extentand
methodsofinspectionforincorporationintorequisitedesigndevelopmentandmaintenanceplans.
Theprogrammeincludes:

Materialprocurement,

Manufacture,[Seealso:Chapter8].

Assembly,

Operation,

Testprogrammes.

[Seealso:ECSSEST30series;ECSSEST3201forfracturecontrol]

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34.3.1.2

Programme approval

Thecontentsoftheprogrammearesubjecttoapproval,whichcovers:

Thenature,sizeanddistributionofdefectscoveredbyparticularinspectiontechniques,[See:
33.2fortypicaldefects].

Theabilitytoapplyintendedmethodsforeveryfracturecriticalitem,FCI,configuration.

InitialinspectionofallfinisheditemsbytheNDImethodrelevanttotheassumedinitialdefect
ordamage.NDIisperformedforthetotalitem,eventhoughonlyonelocationisanalysed.

Inspectioncanbenecessaryforlimitedlifeitems.

Verificationofthestructuralredundancyforfailsafeitemsbeforeeachflight.

PosttestNDIforallprooftesteditems.

34.3.2

Repairs

Repair procedures also need analysis and test to demonstrate that they are able to restore the
structuretoaflightworthycondition,[Seealso:Chapter41].
Repairproceduresarealsoaccompaniedbynecessaryinspectionforsubsequentoperationaluse.

34.4

Inspection

34.4.1

Basic considerations

34.4.1.1

Manufacturing

Tolimitthenumberofscrapitems,someinspectionandtestingcanbeperformedatanearlystage
of manufacture. However, some inspection or testing can be performed only on completely
assembledelements,e.g.prooftesting.

34.4.1.2

Damage

Thepossibilityofhumanintroduceddamageduringlateractivities,e.g.integrationandacceptance
testing,alsoneedstoberecognised.Thefactthatdamagecanoccurduringcheckoutandoperation
isagoodreasonfornotreducing,belowacertainlevel,thesizeofdefectsthataredetected.

34.4.1.3

Inspection techniques

Acombinationofdifferentmethodsislikelytobeneededinordertodetectallofthedefectsthatare
identifiedasintolerable,e.g.:

UltrasonicC-scanstodetectdelaminations,and

Xraytodetectgaps,foreignparticlesandseriouslevelsoffibrebreakage.

34.4.1.4

Damage tolerance

Inviewofthedifficultyofdetectingdefects,itisoftenmoreeconomictodesignaCFRPitemtoa
relatively higher damage tolerance than stated initially. This does not necessarily result in higher

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massesifthenotchsensitivityofthematerialandlaminateconfigurationisevaluated,selectedand
controlledaccordingly.

34.4.1.5

Design strategy

The design strategy balances the differing requirements arising from the inevitable conflicts
between,e.g.:

Structuralperformance,

Lowmasses,

Sensitivityofelements,

Economicmanufacturing,

Lowscrap,and

Repairrates.

Nondestructiveinspection(NDI)is,inthisrespect,asynonymforasetofcontrolactivitiestailored
toachievethenecessaryquality.
Thekeyelementsandthelevelofcontrolaredeterminedbythedesigner.

34.5

Definition of inspection procedures

34.5.1

Procedures

34.5.1.1

General

Theinspectionproceduresaregeneratedandtheirsensitivityverified,Ref.[341].
Generalinspectionproceduresarereviewedwithrespectto:

Theirapplicability,

Theknownconstraints,

Theprovisionsnecessary,

Whetherornottheyneedtobeadaptedtoaparticularelement,

34.5.1.2

Sensitivity

Theexpectedorrequiredsensitivityisestablishedconsidering:

Limitedaccess,e.g.tocavitiesinsidestructures.

Disturbancesoftransducers,e.g.atfreeedges.

34.5.1.3

Calibration

AllNDItechniquesarecalibratedtodefinedstandardsatregularintervals,duringthe:

Verificationprogramme,and

Useofequipment,e.g.testcouponswithknownpositionsandsizesofrepresentativedefect
typesfortheitemsundertest.

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34.5.2

Thin composite laminates

Abasicprocedureisproposed,Ref.[341],tosimplifythesituationforthethinlaminatestypically
used in spacecraft, e.g. less than 2 mm thick, such as shells or facings of sandwich panels. This
comprisesof:
a.

Defineadequatemanufacturingprocesscontrols,including:
1.

materialsensitivitytonotches,

2.

accuratelaminateconfiguration,

3.

adequatecuringprocessing.

Preferably this is accomplished by nondestructive methods or by those techniques that record


resultsautomatically.
b.

Design the structure withanallowablestress or strain reflectinga circular hole through the
thicknessof,say,6mmdiameterandacirculardelaminationof,say,12mmdiameter.

c.

Select NDI methods, procedures and criteria capable of reliably detecting defects of the
selectedsizes,evenifsurfacedefectsconsistofscratchesthroughoneplyonlywithalength
oftheassumedhole.

d.

Considertheneedsfortheinspectionofjointsseparately,e.g.holesandadhesivebonds.

e.

Acceptallhardwareinspectedandfoundwithoutindicationsunderthedefinedcondition.

f.

Wheredeviationsarepresent,assessalloccurrenceswhichexceedthesetcriteriacasebycase
byapplyingestablishednonconformanceprocedures.

34.5.3

Thick composite laminates

Thickerlaminates,e.g.greaterthan2mmthick,needspecialconsideration,astheyusuallydonot
complywiththeassumptionofathroughthethicknessholeenvelopingtheactualdefect.
Thick composites imply the presence of high loads and multiple lamina. Inspection techniques
capableofdetectingdefectsatalldepthswithinthecompositeareused.

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34.6

Non-destructive inspection techniques

34.6.1

Introduction

Nondestructivetesting,NDT,hasanimportantroleintheapplicationofcompositesandadvanced
materials to space structures, Ref. [342], [343]. Initially, the development of NDT techniques was
driven by the need to detect defects and anomalies in new materials, such as CFRP. This was
influenced by uncertainty as to the significance of defects in structures and a wish to detect all
identifiable features. With a better understanding of material capabilities, further development of
NDTtechniquesisaimedatthosedefectsknowntobesignificantinstructuralintegrity.
NDT technologies are closely associated with the demands of aircraft inspection, Ref. [344]. The
spaceindustrybenefitsfromthisbymodifyingtechniquestosuittheneedsofspaceprogrammes,be
itforlaunchers,satellites,spacestationsorspaceplanes,Ref.[345].
Thereisonerulewhichappliestoallaerospaceprojects:

All structures should be designed and manufactured in such a way that they
can be inspected, both during production and once assembled.

34.6.2

Damage tolerant designs

Inadamagetolerantapproach,flawsareassumedtoexistinfracturecriticalcomponents.Aspartof
thisapproach,factorstobeevaluatedinclude:

Thecriticalflawsizethatresultsinfailureofacomponentwhensubjectedtoknownservice
stressandtemperatureconditions.

Thegrowthrateofsubcriticalcracksandconsequentlythetimethatacomponentcontaininga
subcriticalflawcanoperatesafelyinservice.

The inspection performed to detect defects before catastrophic failure of the component
occurs.

The assumed initial flaw size is based on the intrinsic material flaw size distribution and the
manufacturinginspectioncapability.Formanufacturing,aninspectionreliabilityof90%probability
ofdetection(POD)atthelowerbound95%confidencelevelisgenerallyacceptedfortheassumed
flaw sizes. These flaw sizes are intended to represent the maximum size of damage that can be
presentinacriticallocationaftermanufactureandinspection,Ref.[342].

34.6.3

Advances in NDT

It is widely accepted that more than one NDT technique is needed to detect all possible defects,
anomaliesanddamagepresentwithinanassembledstructure.

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Tocontrolinspectioncosts,itisprudenttousethesmallestnumberofNDTtechniquesnecessaryto
detectcriticaldefects.Greateremphasisisplacedonusingrapid,automatedinspectionsystems.The
moretraditionalultrasonic,radiographicandholographictechniquesarenowbeingcomplemented
bynewertechnologies,suchaslaserbasedultrasonicsorshearographyandcomputertomography.
DevelopmentinNDTisdrivenby:

Availabilityofcheap,powerfulcomputers,

Digitalsignalprocessing,

Imageenhancementtechniques,

Realtimeimageprocessingandpresentation,

Needforlargeareascanningsystems,e.g.forageingaircraft,

Rapidinspectionofaircrafttosavecosts.

Theadvantagesgainedfromthenewdevelopmentsinclude:

Systemautomationandimageprocessing.

Noncontactandnoninvasiveinspection,[Seealso:34.10].

Inspectionofthicksectioncomposites.

Highresolutiontechniquesforpolymer,metalandceramicmatrixcomposites.

Increasedavailabilityofpowerful,portableinspectionsystems.

Automated systems can reduce inspection costs by reducing inspection time and operator
intervention. This applies when the test requirements and sequence has been established and
verifiedforeachitemorstructure,Ref.[3491].

34.6.4

Techniques

34.6.4.1

General

Thereisnowawiderangeofinspectionsystemsbasedonavarietyofprinciples;eachperformsa
differentfunction.Inbroadterms,thetechniquescanbegroupedasbeingapplicableto(someNDT
methodscanbeappliedinbothgroups):

laboratory (L) and production (P) environments for the examination of components and
assembledstructures.

inservice(S)environmentsfortheexaminationoffullyassembledstructures.

34.6.4.2

Laboratory and production based NDT

Forcomponentandassembledstructures,thetechniquesavailableinclude:

C-scanultrasonics,bothconventionalandaircoupled,[See:34.10].

Holography,[See:34.13].

Radiography,[See:34.16].

Computertomography,[See:34.17].

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Lasershearography,[See:34.14].

Thermography,[See:34.15].

34.6.4.3

In-service based NDT

Thetechniquesforfullyassembledstructuresinclude:

Portableconventionalandaircoupledultrasonics,[See:34.10].

Eddycurrents,[See:34.18].

Lasershearography,[See:34.14].

Thermography,[See:34.15].

34.6.4.4

Other techniques

Techniquesthatprovideasupportingroleinclude:

Visualinspection,[See:34.9].

Cointapping,[See:34.9].

Dyepenetrants,[See:34.9].

Resonancebondtesters,[See:34.9].

Acousticflawdetectors,[Seealso:34.20]

Acousticemission,[See:34.11].

34.6.5

Smart technologies for condition monitoring

Easyaccesstocomputingpowerinitiatedthedevelopmentofinspectionsystemsthatareintegrated
into structures to provide continual monitoring of the thermal and strain responses.Such systems
areequallyapplicabletoinservicedamagedetection.

[Seealso:Chapter92forpotentialspaceapplicationsofsmarttechnologies]

34.7

Defects and anomalies for detection

34.7.1

General

NDIcanbeappliedatanytimetoassesstheconditionofacomponent,assemblyorstructure,Ref.
[346],[347].Factorstoconsiderinclude:

New composite mouldings are assessed against quality standards that aim to establish
acceptance levels for anomalies, such as voidage, resin content, fibre misalignment and
rucking,presenceofforeignbodies,microcrackingandmissingplies.

Subsequent fabrication stages can introduce the possibility of machining damage,


delaminations, poor hole quality, adhesive bond integrity, missing components, poor
honeycombsplicing,componentmisalignmentandcontinuityofpottingcompounds.

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Sandwich panel constructions and cocuring give rise to greater complexity from a single
mouldingcyclewiththepossibilityforawiderangeofdefectstooccur,includingcoretoskin
disbonds.

Inserviceinspectionismainlyrelatedtoestablishingthepresenceofsignificantdefects,such
asimpactdamage,delaminations,fibrebreakage,disbonds,moistureuptake,waterretention
inhoneycombs.

Inserviceinspectionisonlyappropriatetosomespacestructures.DevelopmentsinNDTaremainly
associatedwithinspectingaircraft.

34.7.2

Emphasis of NDT development

As composites have become more widelyapplied to aerospace structures,theemphasisplacedon


NDT techniques has changed. The extensive use of sandwich honeycomb constructions, cocuring
and adhesive bonding enables more complex constructions to be manufactured. With these the
factorsofgreatestconcerninclude:

Missingormisplacedmaterialsandsubcomponents,

Disbondsanddelaminations,

Integrityoffixingpointsaroundfastenersandinserts,

Damagefromlowenergyimpacts,between0.5Jand10.0Jtypically,whichcancausebarely
visibleimpactdamage(BVID),Ref.[348].

Wherefeasible,apreferenceisgiventotheuseofnoncontactNDTtechniquesinsteadofthemore
traditionalmethods,Ref.[349].

34.8

Overview of NDT techniques

34.8.1

Selection of NDT technique

Numeroustechniquesareusedfortheinspectionofmaterials,componentsandstructures,Ref.[34
3],[344],[346],[347],[349].
FactorsinvolvedintheselectionofanappropriateNDTtechniqueinclude:

Application:Laboratory,productionorinservice.

Materialstobeinspected.

Componentorstructuredimensionsandgeometry.

Accessibilitytoareatobeinspected.

Abilitytodetectacertaintypeofdefect.

Sensitivitytodefectsize.

Availabilityofreliableequipmentandresources.

Recordingandunderstandingofresults.

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Equipmentcost.

Inspectionspeed,hencecost.

OwingtoalackofstandardisationofNDTtechniques,itiscustomaryforcompositemanufacturers
toselectatechniqueandproveitsacceptabilityforeachcomponentorstructureproduced;provided
thatthedesignhasstipulatedtheinspectionrequirements.

NDI methods which have been applied to aerospace materials and structures are described. The
basic techniques, e.g. ultrasonics, holography and Xray, have been used successfully for many
years. The physical recording media, e.g. film, has evolved to electronic data storage and
manipulation.

34.8.2

Detection of defects

34.8.2.1

General

BasicguidelinesonwhichNDTtechniquescandetectwhichspecifictypeofanomalyordefectare
givenfor:

Manufacturing,assemblyandpayloadintegration,using:

contactmethodsinTable34.8.1

noncontactmethodsinTable34.8.2

Inserviceforlonglifestructures,using:

contactmethodsinTable34.8.3

noncontactmethodsinTable34.8.4

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Table34.81DetectionofmanufacturingdefectsbycontactNDTtechniques
Defect

Porosity
Prepreg
gaps
Contaminat
ion (solid)
Contaminat
ion
(backing
sheet)

Visual
Inspection
Only
possible on
outer
surface
Successful
on outer
surface
Successful
on outer
surface
Detection
only
possible in
thin
laminates

Tap Test

Ultrasonic
C-Scan

Acoustic
Flaw
Detector

Fokker
Bond
Tester

Eddy
Current
s

Acoustic
Emissio
n

NS

Successful

NS

NS

NS

NS

NS

Successful

NS

NS

NS

NS

NS

Success is
particle size
dependent

NS

NS

Only if
metallic

NS

Detection
only
possible in
thin
laminates

Successful

Successful

Successful

NS

NS

NS

NS

Detection
Possible

NS

Fibre
alignment
lay-up
order

Detection
on outer
surface

NS

Detection of
lay-up order
possible
using pulse
echo

Fibre/resin
ratio
variations

NS

NS

Detection
possible

NS

NS

Detection
Possible

NS

Prepreg
joints
Interply
delaminati
ons
Microcrack
ing
Skin to
core
debonding

Successful
on outer
surface
Possible on
thin
laminates

NS

Detection in
thin
laminates

NS

NS

Detection
Possible

NS

Possible on
thin
laminates

Successful

Good
detection

Good
detection

NS

Detection
Possible

NS

NS

Detection
Possible

NS

NS

NS

Detection
Possible

Outer
surface
disturbance
can be
visible

Successful
for thin
skins

Successful

Good
detection

Good
detection

NS

Detection
Possible

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Table34.82DetectionofmanufacturingdefectsbynoncontactNDTtechniques
Defect

X-ray
Radiography

Holography

Porosity

Successful

Prepreg gaps

Successful

Contamination (solid)

Successful

NS
Successful,
mainly on
thin
laminates
NS

Contamination (backing
sheet)

Not suitable

Successful

Successful

Detection
possible

Detection
possible

Prepreg joints

Thermography

Laser
Ultrasonics

Air-coupled
Ultrasonics
(1) (2)

Computer
Tomography

Laser
Shearograph
y
NS

NS

NS

Successful(1)

Successful

NS

NS

Detection
Possible(1)

Successful

Detection
possible on
thin laminates

NS
Possible
detection in thin
laminates

NS

? (1)

Successful

NS

Detection
Possible

? (1)

Detection
Probable

Detection
Possible

NS

NS

NS(1)

Successful

Detection
Possible

NS

NS

NS

? (1)

Detection
Possible

NS

Successful

Detection in
thin
laminates

Detection
Possible

NS

? (1)

Successful

Interply delaminations

NS

Successful

Detection
Probable

Detection
Possible

Successful(1)

Detection
Probable

Detection
possible on
thin laminates
Detection
Probable

Microcracking

On edges with
penetrant
enhancement

NS

NS

NS

Detection
Possible(1)

NS

NS

Skin to core debonding

NS

Successful

Detection
Probable

Detection
Possible

Successful(1)

Detection
Probable

Detection
Probable

Fibre alignment
lay-up order
Fibre/resin ratio
variations

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Table34.83DetectionofinservicedamagebycontactNDTtechniques
Acoustic
Fokker
Visual
Ultrasonic
Defect
Tap Test
Flaw
Bond
Inspection
C-Scan
Detector
Tester
Detection
Matrix Microcracking
NS
NS
NS
NS
Possible
Only on
Possible if
Delaminations
Successful
Successful
Successful
surface
severe
Detection
Only on
Broken Fibres
NS
NS
NS
surface
Possible
Detection
Possible if
Crushed Core
NS
NS
NS
severe
Possible
Possible if
Possible if
Skin:Core Debonding
Successful
Successful
Successful
severe
severe
Possible if
Possible if
Skin Debonding
Successful
Successful
Successful
severe
severe
Water in sandwich
Detection
NS
NS
NS
NS
panels
Possible
Key: NS - Not Successful.

Eddy
Currents

Acoustic
Emission

Only if
Severe
Detection
Possible

Detection
Possible
Detection
Possible
Detection
Possible

NS

NS

NS

NS

NS

Detection
Possible

NS

NS

NS

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Table34.84DetectionofinservicedamagebynoncontactNDTtechniques
Defect
Matrix
Microcracking
Delaminations
Broken Fibres

X-ray
Radiography
Possible on
edges with
penetrant
Detection
Possible
Detection
Probable

Crushed Core

Successful

Skin:Core
Debonding

Detection
Possible
Detection
Possible

Skin Debonding
Water in Sandwich
Panels

Successful

Key: NS - Not Successful;

Holography

Thermography

Laser
Ultrasonics

Air-coupled
Ultrasonics(1)

Computer
Tomography
(if available)

Laser
Shearography

NS

NS

NS

Detection
Possible

NS

NS

Detection
Probable
Detection
Possible

Detection
Possible
Detection
Possible

Detection
Possible

Successful

Detection
Probable

Detection
Possible if severe

NS

Detection
Possible

Successful

Detection
Probable
Detection
Probable

Detection
Possible
Detection
Possible

Successful

NS

Successful
Detection
Possible
Detection
Possible if
severe
Successful
Successful
Detection
Possible

Successful
Successful
Detection
Possible

Detection
Probable
Detection
Probable
Successful

Detection
Probable
Detection
Possible
Detection
Possible if
severe
Detection
Probable
Detection
Probable
Detection
Possible

? - To be determined; (1) AIRSCAN, [See also: 34.10]

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The size and shape of defects detectable by a particular technique depend on the nature of the
materials under test, the structural configurations and the equipment used, e.g. probe type, test
frequency, resolution of the scanning mechanism and recording media. It is therefore impossible to
statedefinitedetectionlimitsforaparticularNDItechniquebecauseeachisapplicationdependant.

34.8.2.2

Contact versus non-contact methods

Contact methods are those techniques where there is a physical interaction with the component or
structurebeinginspected.Thisincludes:

Humancontactwiththestructureduringinspection.

Manualoperationofprobes.

Useofwaterorgelcouplants,includingwaterimmersion.

Rollerprobes.

Directmechanicalloading,asinacousticemission.

Applicationofsurfacecoatingsorpenetrantstohighlightdefects.

Any contact with a material introduces the possibility of contamination, which is undesirable for
spacepayloads.Noncontacttechniquestendtolimitcontaminationsources.
Those techniques reliant on manual operation can introduce uncertainties regarding operator
consistency and possible error. If human judgement is used to interpret the significance of a signal
reading,thiscandifferbetweenindividuals.Tolimitanysuchinconsistencies,operatorsareprovided
withtrainingtoparticularindustrystandards.
Automatedsystemsaimtoovercomeanyhumanoperatorrelatedinconsistencies.Theytendtoneed
extensivesetupandfinetuningbyqualifiedengineersinordertoprovidesufficientconfidenceinthe
results produced, especially when compared with manual techniques. It is also not uncommon for
newautomaticsystemstoproducelargenumbersoffalseindicationsduringthesetupphase.
Electronicstorageoftheinformationobtainedduringinspectionenablessignaldataandimagestobe
compared or enhanced when specific features are being addressed. Historical comparisons are also
feasiblebetweencomponentsmadeatdifferenttimes.Suchrequirementstendtofavournoncontact
techniques, where the object can be scanned and rotated during examination to show different
orientations.

[Seealso:34.9Contacttechniques;34.10Ultrasonicaircoupledtechniques]

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34.9

Traditional contact NDT techniques

34.9.1

General

Eachtechniqueiscodedassuitableforapplicationinthelaboratory[L],duringproduction[P]orin
service[S]duringtheperiodicreexaminationofacomponentorstructure.

34.9.2

Visual inspection

VisualinspectionistheoldestandmosteconomicalformofNDT.Itiswidelyusedforlocatingdefects
anddamageon,ornear,thesurfacesofmaterialsorcomponents.Somelevelofcontactisnecessary,
e.g.bytheinspectortouchingtheitem,althoughnoadditionalchemicalsubstancesareused.
It enables a rapid survey of large areas, or a detailed examination of small areas using optical aids
suchasmagnifyinglenses,borescopesandendoscopes.Visualinspectioncanbefollowedbyanother
typeofNDTinspectiontoquantifythesizeofasubsurfacedefect.
Application:[L,PandS]Contactornoncontact.

34.9.3

Dye penetrant

In this technique a liquid dye is applied to the component surface, and is trapped by any surface
breaking defects. The component is then cleaned, but some of the dye is retained in the defects
present.Thisisthenabsorbedbyadevelopingagenttoproduceacontrastingstainwhichindicates
thepositionofadefect.DyescanbecolouredorfluorescentunderUVlight.
Application:[L,PandS]Contact.

34.9.4

Magnetic particle

A magnetic field is generated in the component. Any surface defects or nearsurface cause field
leakage and preferentially attract the applied magnetic particles. The particles are normally in the
formofasuspensionofmagneticironoxidepowderinahydrocarboncarrierfluid.Themagneticfield
isinducedbymagnetsorappliedfluxorcurrent.Ingeneral,defectsareorientedacrossthemagnetic
field to be detectable, with subsurface defects detectable if their size and position is sufficient to
disturbthefield.
Application:[L,PandS]Contact.

34.9.5

Mechanical resonance or impedance

Thetypesoftechniquesthatcanbeclassedasmechanicalresonanceorimpedanceinclude:

Taptestingisoftenconductedalongwithvisualexaminations.Componentsaretappedwitha
coin or special hammer. Variations in sound (resonance) between good and bad areas are
usually detected by the operator hearing the differences. Tap tests have a rather limited
sensitivity, but can detect fairly large delaminations under the right conditions. It is also
difficult to assess which areas have or have not been tested, given a particular area to be
screened.

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Bond testers measure mechanical impedance under high frequency oscillation. It compares
goodwithbadareas,providingdataonthecohesive,butnottheadhesive,natureofthebond;
exceptintheextremecaseofnoadhesion,[See:34.20].

Acousticflawdetectorsworkonasimilarprincipletobondtesters.

Application:[L,PandS]Contact.

34.10

Ultrasonic techniques

34.10.1 Introduction
34.10.1.1 General
Therearealargenumberoftechniquesknowngenerallyasultrasonicwhichcanbeappliedinthe
laboratory, in production and inservice. Each has their strengths and weaknesses, so for any given
circumstancesonecanbemoreappropriatethantheothers.
Mosttechniquesinvolvesomecontactwiththecomponentorstructure,butaircoupledsystemsaim
toavoidcontaminationofcomposite,spacedestinedstructuresbywaterorgelbasedcouplants.This
noncontacttechniquewasevaluatedbyAleniaforCFRP,Ref.[3494],andwasselectedbyFokkerto
inspectsolarpanelsubstrates,Ref.[3491].
Ultrasonic testing uses highfrequency sound waves; often in the kHz to MHz range. The sound
energy is reflected or scattered by defects lying within the sound path. The principal relies on
transducers,or probes, toemit and receive sound.The orientation of transducers in relation to both
thestructureandthedefectsdetermineswhichfeaturesaredetectedandresolved.Thepresentationof
signalresponsesinCscanformrepresentsthebaselinemeansofexaminingmaterials.Ithasbecome
theacceptedmeansofinspectingcompositesowingtoitsversatilityindetectingdefects,Ref.[343],
[3410].
ConventionalCscanultrasonicsisbynomeansanidealmethodasitneedsacontactpathbetween
thetransducerandthecomponentundertest,usuallyachievedbyuseofliquidcouplant.Toinspect
largeareas,theprobesaregenerallymovedusingamechanicalscanningdevice.Thiscanbelargeand
complexinordertoinspectcontouredsectionsofaircraftmadefromcomposites,Ref.[3495].
As the name suggests, aircoupled ultrasonics do not use couplants, but rely on air transmission
betweentheprobesandthecomponentundertesttobothsendandreceivetheultrasound.

34.10.1.2 Sound waves


Composites are anisotropic (fibre and resin), orthotropic (variable fibre orientation) and laminar in
construction. The location, alignment and orientation of potential defects varies accordingly. It is
therefore necessary to utilise different soundwavebehaviours in composites to enable defects to be
detectedindifferentconstructions.
Awaveisatransienttimeandpositionphenomenonwhichconveysenergythroughspace.Thespeed
ofasoundwave(timeofflight)andthestrength(energy)aretheparametersusedforlocatingdefects
andquantifyingtheirsize.ThewavebehaviourswhichareutilisedinNDTare:

bulkwaves(planeorspherical),e.g.longitudinalwaves

transversebulkwaves,e.g.shearordistortionalwaves

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surfaceeffectsnearaboundary,e.g.Rayleighwaves.

plateeffects(inamediumwithtwoparallelboundaries,i.e.alaminate),e.g.Lambwaves,Ref.
[3411],[3412].

34.10.2 Modes of examination


Ultrasonicequipmentisusuallyconfiguredtooperateinoneofthreemainmodes,i.e.:

Throughtransmission(T-T);usingtwotransducersplacedonoppositesidesofthecomponent.
Onetransducersendstheultrasonicpulse,theotherreceivesit.

Pulseecho (P-E); using one transducer placed normally (longitudinal waves) or at a selected
angle (shear waves) on the component surface. This single transducer both sends and then
receivestheultrasonicpulse.Sometechniquesalsouseareflectorplateplacedonthebackface
ofthecomponent.

Resonance or resonant frequency; by creating a continuous ultrasonic wave in the material.


Sensingthereceivedsignalphase,amplitudeorresonantfrequencyshiftindicatesthematerial
impedanceorstiffness.

ThesemodesarethebasisforthewellestablishedandprovenformsofultrasonicNDT.
Acouplantmediumisnormallyusedtoensureagoodacousticpathbetweenthetransducersandthe
component. Alternatively the component and transducers are completely immersed in a suitable
couplingliquid,e.g.water.

34.10.3 Ultrasonic signal presentation


Whenacomponentisexamined,theultrasonicsignalispresentedinvariousformsforinterpretation.
Theseare:

A-scan:Asinglepointsignaldescribingtheultrasonicresponseofmaterialimmediatelybeneath
thetransducer.

B-scan:Ascannedlineshowingfeaturesatidentifiabledepths.

C-scan:Anareascanshowingvolumetricdefectsinthematerial.

34.10.4 Data and image processing


ImageenhancementtechniquesareinvaluabletoolswhenappliedtotheinterpretationofCscans.The
useofimageenhancementenablesthedisplayoffeatureswhichcannotbeviewedwhenanultrasonic
Cscanisinitiallyformed,Ref.[3410],[3489].Postprocessingofdatacaninclude,Ref.[3489]:

Imagepresentation:

Lookuptablesandcolourcoding.

Imagereversal.

Greyscalerampingorsawtoothscaling.

Isometricprojection.

3Dimaging.

Binarydisplayimaging.

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Imagehistogramevaluation:

Imageenhancement.

Equalisationenhancement.

Logarithmicforcingfunctions.

Windowingandlevelslicing.

Subareaevaluation.

Kernelmultiplications:

Loworhighpassfilteringandsmoothing.

Selectiveorientationfilteringandshadowing.

TwodimensionalFourieranalysis:

Fibreorientationdistribution.

Effectsofpixelsizes.

Imageenlargement.

Maskmultiplicationfiltering.

Fullvolumeimaging:

3Ddatabases.

Peakamplitudeimages.

Integratedamplitudeimages.

Statisticalimaging.

Frequencydomainimaging.

3Dpresentation.

Data processing is not only useful forultrasonics but is equallyapplicable toother NDT techniques
producingdigitaldata.

34.10.5 Equipment calibration


Ultrasonicequipmentneedscalibrationtoensureconsistentandreliabledetectionofdefects.Thiscan
beachievedusingreferencespecimenscontainingdefectsofknowndimensionsandlocations.
Withultrasonicstherearemanypossiblesoundwavemodes,transducertypesandfrequencyranges.
Asystematicmeansofdescribingandcomparingtechniquesanddevicescanbeuseful.Thereceiver
operating characteristic, ROC, is one such means, Ref. [3413]. The ROC method assesses the
performanceofasystemandshowstheprobabilisticcharacterofdefectdetection.Itisbasedonthe
generaltheoryofsignaldetectionbycountingtheinputandoutputfromadiagnosticsystemwhich
includesthetaskofseparatingasignalfrombackgroundnoise,Ref.[3413].

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34.10.6 Large area scanning


There are several means of scanning components and mouldings by passing a transducer over the
surfaceofinterest,Ref.[3411],[3414],[3495]:

XYZscanningframesfor:

smallindividualcomponents

largeaircraftsections,Ref.[3495].

XYscanningframesforflatpanels.

Programmableroboticsforrepetitivetesting.

Thetypesoftransducersusedinclude:

Rollerprobesformainlyflatconstructions.

Waterjetprobesforshapedmouldingswithcutouts,Ref.[3495].

Aircoupled probes for CFRP composites and solar panel substrates, Ref. [3491], [3492], [34
94].

To reduce the time to inspect large areas, such asaircraft, portablescanning systemsarenow being
introduced, Ref. [3415], [3416]. Examples include LACIS large area composite inspection system
andMAUSmobileautomatedultrasonicscanner.Themainfeaturesoftheseare:

Use in pulseecho (depth and amplitude), ultrasonicresonance and eddycurrent modes, i.e.
interchangeable.

Multipletransducers,givingstripcoverageviasimpleoscillatorymotionofeachtransducer.

Portable,wheeledscannerwithautomatictransduceralignmentforcontourfollowing.

Manualoperationofscanner.

Waterdropcoupling.

AutomateddatacollectionandenhancedCscanimagingthroughalaptopcomputer.

Scanratesofupto9m2perhour.

The LACIS or MAUS derivatives are used principally for detecting impact damage and bondline
defects.

34.10.7 Acousto-ultrasonics
Also known as the stresswave factor method (SWF), acoustoultrasonics uses stochastic wave
propagation to detect and quantify defect states, damage conditions and variations of mechanical
propertieswithincomposites,Ref.[3410].
Itisnotnecessarilyintendedtoresolveeachindividualflaw,butinstead,toassessthecollectiveeffect
of diffuse flaw populations. Accordingly, the SWF approach was devised to evaluate the integrated
defect state due to porosity, matrix crazing, fatigue damage, fibre bunching, fibre breaks, resin
richness,poorcuringorpoorfibretomatrixbonding.

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SWF can be described as a generalised approach to ultrasonic testing using two probes (transmitter
and receiver). The received signal is a result of multiple interactions within the material
microstructure,i.e.multiple,reflected,scatteredandmodeconvertedwaves.
Signal interpretationisall important.With sufficient correlation with measured properties from test
coupons,itisindicatedthatSWFiscapableofquantifyingresidualultimatetensilestrengthoffatigue
damagedcomposites,interlaminarshearstressandadhesivebondstrength.

34.10.8 Lamb wave (guided wave)


34.10.8.1 General
Lamb waves are capable of propagating relatively long distances in thin plate geometries and
laminatedstructures.LambwavesofferapotentiallypowerfulNDEtechniqueforassessingthehealth
of such structures. Lamb wave propagation properties strongly depend on the thickness and the
mechanical properties of the material. Changes in the effective thickness and material properties
caused by structural flaws, such as disbonds, Ref. [34104], [34105], [34106], corrosion, and fatigue
cracks,canbedetectedefficientlybymeasurementsofvariationsinLambwavepropagation.Owing
tothestrongdispersionoftheLambwavemodes,thepropagationvelocityisacharacteristicfunction
oftheproductoftheimposedacousticfrequencyandtheeffectivethicknessofthematerial.
Lamb wave techniquesare envisaged for health monitoring to detect damage in composite material
(diagnosis based on Lamb wave propagation analysis) using a permanently attached guided wave
array, Ref. [34107], [34108]. By taking measurements at different stages in the life cycle of the
structure, using a permanently attached device on the structure, comparative measurements can be
performedtodetectemergingdefects.
Several researchers have shown that Lamb waves are viable in principle, but have limitations,
including:

strongsensitivitytothematerialproperties,

thicknessesoftheadherends,

relativeinsensitivitytodefectsatthebondlinelayer.

Embedded modes, which propagate along an embedded layer, are largely insensitive to the
adherends. The dispersion curves show a major improvement in sensitivity to the properties of the
layerandtotheboundaryconditionsbetweenlayerandtheadherends.Thedifficultyistogenerate
thesespecificmodes,socurrentapplicationsarelimitedtohomogeneousandisotropicmaterials,e.g.
adhesive bonding with thin metallic plates or glass. Although attempts have been made with
compositematerials,thetechniqueremainsalaboratoryresearchtool.Asignificanteffortisneededto
modelthephenomenatoaccountforvariationsinmaterialpropertiesinordertomeetindustryneeds.
Conventionalmethodsofexcitinganddetectingguidedwavesincludetheangleincidencetechnique,
interdigitaltransducers(IDTs)andEMATs.

34.10.8.2 Leaky-Lamb-wave techniques


Lambwavesoccurinplatesasaresultofreflectionsbetweentheadjacentsurfacesfoundinlaminates.
In some instances, these waves can be used when more conventional techniques, such as a single
probepulseechomodefailstolocatedefects.LeakyLambwavesarealsotermedobliquelyinsonified
ultrasonicwaves,Ref.[3417].

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Inthistechnique,accesstothecompositeisonlyneededfromoneface.Forthickcomposites,e.g.30
plyCFRP,itcanbedifficulttoresolvedelaminationsinthefirstfewplies.Byusingatransmitterand
receiver, 10mm apart, it is feasible to detect nearfield, subsurface defects, Ref. [3411]. The basic
equipment used can be the same as that used in normal contact pulseecho mode. This can be a
commercialbroadbandprobewithadigitalultrasonicflawdetector.
The utilisation of Lamb waves is seen as a lowcost means of inspecting large structures for
delaminations,Ref.[3418].Byplacingatransmitterandreceiveradjacenttoeachotheronthesurface
ofacomposite,itisfeasibletodetectdefectsbycomparingoutgoingandreflectedsignals,asshownin
Figure34.10.1,Ref.[3412].Thetransmitterandreceiverarelocatedatapoint,buthavetheabilityto
inspect the surrounding composite when rotated or line scanned. It is possible to detect 20mm
delaminationsatadistanceofupto500mm.

Figure34.101LeakyLambwavetechniqueforcomposites

34.10.9 Rayleigh wave techniques


Rayleigh waves are not applied to polymer composite examination. They are more appropriate for
ceramiccompositesandcoatings,Ref.[349].

34.10.10 Backscattering techniques


Theseare capable of detecting matrixcracking, porosity, fibre orientation and fibre misalignment in
individualplies,Ref.[343],[3420].Thetechnique,asshowninFigure34.10.2,enablesatransducerto
berotatedaboutanormaltothesurfaceaxisatvariousanglesofincidence,Ref.[343].Themaximum
backscatteredenergyisreceivedbythetransmitting/receivingtransducerwhenthetransduceraxisis
normaltothedefect.Thus,theshape,locationandorientationofthedefectcanbeapproximatedby
measuringthepulsesignalamplitudeasafunctionofrotation(polar)angle.

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Figure34.102Detectionoffibreorientationbybackscatteringmeasurement

34.10.11 Transducer technology


34.10.11.1

General

Transducers, or probes, emit the ultrasonic waves into the subject material or receive the resulting
signal.Insomesystemstheprobescanperformbothfunctions.Theactiveelementwithinaprobeis
usually made of a piezoelectric ceramic or polymer (PVdF). The dimensions of the piezoelectric
elementlargelydefinetheeffectivefrequencyrangeofthetransducer,althoughtheactualoperating
frequency is determined by the signal from the driving electronics. Transducers generally have a
stated frequency value, giving their optimum sensitivity and the centre of their effective frequency
range.
Someofthetransducerandappliedsignalvariableswhichdifferbetweentestingtechniquesinclude:

Focusedorunfocusedprobes.

Ultrasoundfrequency:

selectedwithrespecttomaterial,defectsizeanddefectlocation.

highfrequenciesforbetterdefectresolution.

lowfrequenciesforlowsignalattenuation.

Probealignmenttosurface:

normal,

angled,or

oblique.

Signalpulseprofile:

wavetrain(pulse)duration,

signalenergy.

Modeofoperation,e.g.pulseecho,throughtransmission.

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34.10.11.2

Phased-array transducers

Piezocompositematerialshaveprovidedanewultrasoundprobetechnologyforthenondestructive
testing of materials; known as Phasedarray transducers. The probes comprise a large number of
individualelementseachofwhichcanbedrivenindependently.Thetransducerelementsareusually
organisedinlinear,annular,circularormatrixarrays,asshowninFigure34.10.3.
Phasedarray transducers can be used with conventional coupling agents (gel, water) either as a
contactoranimmersionconfiguration.Intheory,alltheapplicationsusingultrasoundtechniquescan
usephasedarrayprobes.

Figure34.103Phasedarraytransducers:Elementconfigurations
The probes are connected to speciallyadapted drive units enabling independent, simultaneous
emissionandreceptiononeachchannel.Theunitsalsoenabledifferentelectronictimedelaysforeach
channelduringbothemissionandreception.Electronicscanning,focusinganddeflectioncanthenbe
carriedout;asshownschematicallyinFigure34.10.4,Ref.[34101].
Theoretically,alltheapplicationsusingultrasoundtechniquescanusephasedarrayprobes.
Incomparisontoclassicalultrasonictechniques,themainadvantagesofphasedarrayprobesarethe
improvementofinspectionperformances,thereductionofinspectiondelays,andthepossibilityofa
completeinspectionofaniteminonescan.Theconventionalmechanicalscanningisreplacedbythe
much faster electronic scanning (advantage for large structures). Electronic scanning in depth can
becomeinterestingforstructuresoflargethickness.Moreover,electronicfocusingenablestheuseofa
single probe for working at different depths. The electronic focussing can be advantageous for
structuresincludingheterogeneitiesofsmalldimensionstoo.Recentinvestigationshaverevealedthe
capabilityofsuchsensorstodetectfibrewaving.
Electronicdeflectionenablestheangleofincidencetobevariedwithasingleprobegivingaccessto
particular,inaccessibleareasandfacilitatinginspectionofstructureswithcomplexshape.

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Electronic scanning
Groups of elements are sequentially
activated to move the beam along the
transducer (with electronic delays to
focus the group).

Electronic focusing
Electronic delays are applied to each
element to focus the beam.

Electronic deflection
Electronic delays are applied to each
element to deflect the beam

Figure34.104Phasedarraytransducers:Functionality
Advanced functions of ultrasonic phasedarrays are emerging for the nondestructive testing of
aeronautic parts, increasing further thepotential benefits of the technology, e.g. for emission: multi
beam generation; for reception: differentiated sum of elementary signals, for emissionreception:
iterativeprocess.
Currently available phasedarray transducers are expensive, mainly because MHzorder frequencies
imply tight tolerances and high manufacturing precision. Ongoing work aims to develop cheaper,
lowfrequencyphasedarraysystemsfordamagedetectioninaircraftstructures.
Theinitialapplicationsofultrasonicphasedarrayprobeswereforcomplexshapedstructures(areas
with difficult access) and in the metallurgic field (to reduce control delay by electronic scanning).
NASA,McDonnellDouglasandBoeingSpacehaveusedphasedarraytechnologyfortheinspection
ofweldedspacestructures,e.g.frictionstirwelds(DeltaIVtank)andlaserwelds.Thetechnologyhas
beenappliedsuccessfullytolargeaeronauticstructuresmadeofcompositematerialsandhoneycomb
parts(industrialisationofthephasedarraysystem).
SomeexamplesofthesuccessfulapplicationsofphasedarraytechnologywithintheEuropeinclude
NDToflaserbeamweldingofskinstiffenersforthefuselageofAirbusA318(StNazaire)andforthe
inspectionofcompositepartsofAirbusA380(Nantes).

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34.10.12 Air-coupled techniques (non-contact)


34.10.12.1

General

Theuseofliquidcouplantshastraditionallybeennecessarybecauseofthesoundsignalattenuation
caused by air at high frequencies, e.g. MHzrange. Strong reflections at the interfaces between
transducertoairandairtomaterialundertestproduceveryweaktransmittedsignals.Advancesin
acoustic transducer matchingtoair technology in combination with tone burst excitation offer the
opportunityforaircoupledultrasonics,Ref.[3421],[3492].
Aircoupled ultrasonic techniques have become reliable and useful methods for noncontact non
destructivetesting.

34.10.12.2

Applications

Numerous cases exist where coupling agents, such as water, gels, grease, glycerine, are either
prohibited or not desirable, e.g. green powders, uncured polymers, solar panel sandwich supports,
some thermal protection systems sensitive to water ingress, rough surfaces, nonflat surfaces and
porousmaterials,suchasceramicsandcarbon/carboncomposites.
Noncontact transducers have been used for quantitative and qualitative ultrasonic evaluation of a
wide range of materials, including, Ref. [3496], particulate and fibrous multilayer composites,
includingprepregs;compositehoneycombstructures;ceramics(greenandsintered);metal(powder
based);rubbersandplastics.

34.10.12.3

Transducers and configuration

Techniques used in noncontact modes include operation of transducers in throughtransmission,


separatetransmitterandreceiverplacedonthesameside(pitchcatchconfiguration)andrecentlya
singletransducerindirectreflectionmode;asshowninFigure34.10.5.

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TWO-SIDED INSPECTION

Figure34.105Noncontactultrasonics:Aircoupledsensorconfigurations
A broad range of frequencies, typically from 50 kHz to 5 MHz, are possible using different sensor
technologies: piezoceramic, piezocomposite or capacitive transducers, Ref. [3497]. Some of them
provideimprovedfocussingwhichgivesbetterresolution.
Capacitivetype transducers, characterised by high bandwidths, have been used to evaluate
compositesandothermaterials.Theyhavebeensuccessfullyusedforthegenerationanddetectionof
guidedwavesinanisotropicviscoelasticmaterialsinanoncontactmode;asshowninFigure34.10.6,
Ref.[3498].

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Figure34.106Noncontactultrasonics:Capacitivesensorsinplatewave
configurationsetup
Althoughtheapplicationsfornoncontacttransducersatfrequenciesabove3MHzinambientairare
limited, transducers between 200kHz to 3MHz have been used for several applications, including
space,aeronauticalandmedicalindustries.
The availability of various frequencies and digital filters enable an optimisation between high
resolutionforcompositesandhoneycombs,e.g.0.5MHzto1MHz,andhighpenetrationformaterials
suchasfoam,rubberandwood(20kHzto200kHz).

34.10.12.4 Airscansolarpanelsubstrates
Airscan, a commercial system from QMI (USA), operates in throughtransmission or singlesided
inspection (via Lamb waves). It has been evaluated for CFRP structures, some of which contain
highlyattenuativematerials,suchashoneycombsandfoams,Ref.[3494].
Someofthefeaturesofthesysteminclude:

Generaloperatingfrequencyof400kHzor50kHz,Ref.[3492],[3494],comparedwith1MHzor
higherforcontactultrasonictechniques.

Thesignalfrequencycanbealteredforthethicknessofthecomposite.

Awavetrainlikesignalconsistingofupto15sequentialpulses.

Optimisedincidentangleforthetransmittingtransducer.

Superlownoisepreamplificationofreceivedsignals.

TheAirscansystemwasvalidatedbyFokkerasameansofreducingthecostandleadtimeforNDI
ofsolarpanelsubstrates.Figure34.10.7showsaschematicdiagramoftheFokkerfacility,Ref.[3491].

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Qualificationtestshavebeenperformedfor:

ARA(advancedrigidarray)forcommercialgeostationarysolararrays,and

FlatpackdevelopedforEnvisat1.

Each of the sandwich panel constructions is different, notably in their aluminium core cellsize and
thickness.EachhasafurthercomplicationintheformofacocuredKaptonfilmononeoftheCFRP
skinsproviding:

Electricalinsulation(betweensolarcellandsandwich),

Protectionagainstatomicoxygen(Flatpackpanels),and

Thermalcontrol.

Skintocoredisbondsweredetectedinbothtypesofsolarpanelsubstrate,[Seealso:Table34.8.2and
Table34.8.4].ThesystemalsodetecteddelaminationsinCFRPpanels.TheresultsarepresentedinC
scanform.
Furtherstudiesaimtoassessthesuitabilityofthetechniquefortheinspectionofotherflatandcurved
items,e.g.aircraftfloorpanels,antennas,centralcylindersandelectroniccircuitboards,Ref.[3491].

Figure34.107Airscan (air-coupledultrasonics)system:NoncontactNDIof
Fokkersolarpanelsubstrates

34.11

Acoustic emission

AE,acousticemission,isacontacttechniquethatreliesonmechanicalstrainingofthecomponentor
structureundertest.AEcanbeappliedinthelaboratory,inproductionandinservice.
AEtechniquesdetectthesoundsproducedbyastructureasaresultofmechanicalloading,Ref.[343],
[3422].Thesearethenidentifiedandrelatedtocriticalevents,suchasmatrixcracking,delaminations
andfibrefailure.

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DevelopmentsofAEhavemainlyconcentratedontheinterpretationofsignalsandthesignificanceof
noise emanating from stressed components and structures. For composites, some broad comments
include:

Composites under progressively increasing load produce acoustic events at strain levels well
belowtheelasticlimit.

Thepointatwhichacousticeventsbegininrelationtopreviousloadingscanbedescribedasthe
Felicityratio.

Approachingtheelasticlimit,acousticeventsoccurincreasinglyinthesequenceof:

randomlocalmatrixcracking,

transverseplyfailure,

interlaminarshearfailure,andlastly

fibrebreakage.

To enable identification of damage events during the testing or inspection of a structure, the
acoustic signature of each type needs to be known. Such signatures are often material and
structuredependent.Computerpatternrecognitionisimportant.

AE can be applied to proofloaded structures, such as pressure vessels, where the proof test is
obligatoryandhistoricaldataisavailablefromtestingnumerousitems.
Whenstructuresaretestedtoultimatefailureload,AEcanbeusedtoidentifylocaldamageoccurring
prior to final failure. Testing is generally easier with components, where the load application is
usuallysimplerandtheAEresponseeasiertointerpret.
Thetechniquehasbeenevaluatedformeasuringdensityandporosityincarboncarboncomponents,
Ref.[3423].

TheimprovedavailabilityofcheapcomputingpowerhasenabledAEtogaingreateracceptancefor
the inspection of structures. Triangulation methods, by comparison of the arrival time of the same
sound event at several different transducers, locate the positions of acoustic emission sources in
assembled structures, such as aircraft. The frequency and amplitude description of the event is
comparedwithreferencedatatodeterminethetypeofdamage.
AEhasbeenevaluatedforconditionmonitoringsystemsforreusablespacevehiclestructures,suchas
tanks,[See:92.3].

34.12

Laser ultrasonics

34.12.1 General
Laserultrasonicsarenoncontacttechniquesthatcanbeappliedinthelaboratory,inproductionand
inservice.
The development of laser ultrasonic systems was largely in response to a need for noncontact NDI
methodsfortheexaminationofassembledstructures,Ref.[3420],[3424],[3425],[3426],[3427].An
exampleofthistypeoftechniqueisLUISlaserultrasonicinspectionsystemfromGeneralDynamics,
Ref.[3427]andLockheed,Ref.[3428].

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34.12.2 Basic principles


34.12.2.1 General
Figure34.12.1showsanexampleofalaserultrasonicsystem,Ref.[3428].Thesequenceofeventsin
theemissionandreceptionofanultrasoundpulseis:
a.

Ahighpowerlaserpulseisdirectedatthesurfacetobeinspected,typicallyfromaNdYAGor
TEACO2laser.

b.

An ultrasound pulse is generated at the surface, usually by thermoelastic induction (rapid


localisedexpansionbytransientheating)forpolymermatrixcomposites.

c.

The ultrasound response is detected by a second laser operating as part of an interferometer


system.

Figure34.121Laserultrasonictestsystem:Diagrammaticrepresentation
Thebasicmodesofdetectionare,Ref.[3424]:

Optical heterodyning or simple interferometric detection: The wave scattered by the surface
interferes with a reference wave derived directly from the laser.This technique issensitiveto
opticalspeckleandthebestsensitivityisobtainedwhenonespeckleiseffectivelydetected.This
needs a focused beam, enabling the measurement of the ultrasonic displacement over a very
smallspot.

Velocity or timedelay interferometric detection: Based on the Doppler frequency shift


producedbythesurfacemotionanditsdemodulationbyaninterferometerhavingafilterlike
response. This technique is sensitive primarily to the velocity of the surface and is therefore
veryinsensitivetolowfrequencies.Thefilterlikeresponseisobtainedbygivingapathdelay
betweentheinterferingwaveswithintheinterferometer.Twowaveinterferometers(Michelson,
MachZehnder) or multiplewave interferometers (FabryProt) can be used. This technique
enablesmanyspecklestobereceivedandprovidesalargedetectingspot.

Theultrasoundproducedcanbeoftheusualtypes,i.e.longitudinal,shear,plateandRayleigh,Ref.
[3429]. The nature of the ultrasound generated is principally a function of the laser and material
properties,suchasthe:

Laserpulseduration,wavelengthandpulseenergy,

Laserspotsize,

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Thermalpropertiesofthecomposite,

Laserabsorptionpropertiesofthecomposite.

Any inspection system relies ona means of fast optical scanning of the surface to producea Cscan
image. The laser need not be orientated perpendicular to the surface and oblique angles can be
accommodated.
Featuresincompositesthathavebeendetectedusinglaserultrasonicsare,Ref.[3425],[3427]:

Surfacecracks,

Delaminations,

Additionalplies,

Skintocoredisbonds,

Solidcontaminants(backingfilm).

Itisalsopossibletodetectcracksinaluminiumalloysheet,Ref.[3429].

34.12.2.2 Disadvantages
Laserultrasonic techniques generally have a poorer signaltonoise ratio than conventional
ultrasonics,makingdefectdetectionmoreuncertain.Recentimprovementsindigitaldataprocessing
haveaidedthenecessarysignalprocessingandimageenhancementofresults.Prototypefacilitiesare
underdevelopment,Ref.[3428].

34.12.2.3 Applications
Inadditiontotheevaluationofcompositestructure,possibleapplicationsforlaserultrasonicsinclude:

Remoteexaminationforhightemperatureapplications.

Complexshapesandconfinedrecesses.

Remoteanalysisinvacuumandcorrosiveenvironments.

34.13

Holography

34.13.1 Introduction
Holography is a noncontact technique, except for direct vacuum loading that can be applied in the
laboratoryandinproduction.
Itisaprocesswherebyaholographicimageofacomponentissuperimposedonthesamepartwhileit
isstressedslightly.Stressesareinducedbyheating,loadingorvacuumwhichcausedisproportionate
outofplane displacements in defective areas. Discontinuities in the resulting interference fringe
patternscanindicatethepresenceofdefects.
Thetechniquehasbeenappliedtospacestructures,notablysatellites,fromanearlystagebecauseof
its largely noncontact mode of operation. There are now various different versions, which have
benefitedfromtheintroductionofdigitaltechnology,Ref.[3430].Holographycanbeusedtomeasure
accurately small outofplane displacements, to micronlevel resolution, which can be necessary for
antennasundergoingthermaldistortion.

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34.13.2 Laser interferometric techniques


34.13.2.1 General
Therebasictechniqueswhichcanbeusedforinterrogatingastructureare,Ref.[343]:

Interferometry,

Moir,and

Specklephotography.

34.13.2.2 Hologram interferometry


Theoriginalholographictechniquereliedonasplitbeamofcoherentlight(laser),onepartreflecting
offofanobjectandinterferingwiththesecondpartonaphotosensitiveplate.Thehologramproduced
preserved all of the information regarding both the amplitude and the phase of the recorded light
wavefront.Acomplete,threedimensionalreconstructionoftheoriginalimageisthenpossible.

When viewing the stressed object and superimposed unstressed hologram, distortion fringes are
producedwhichdifferwiththeappliedload.Insuchcases,thehologrambehavesinthesamewayas
an interferometer. Controlling the distortion yields a tool that can be used for interferometric
measurements.
The interference fringe patterns can be observed in real time or as a double exposure, where the
featuresofeachcanbesummarisedas:

Realtime:Precisealignmentofanunstressedholographicimagewiththestressedobject.These
interfere, and displacements can be detected of orders of magnitude of the wavelength of the
employedlight.Anychangeinthestateoftheobjectssurfacecausesasimultaneousalteration
ofthefringesystem,hencethetermrealtime,Ref.[3432].Thistechniquedoeshoweverneed
ahighdegreeofprecisionandvibrationcannotbetolerated.

Doubleexposure:Thisissimpler,asasingleholographicplateisusedtomaketwosuccessive
exposuresoftheobject,beforetheplateisdeveloped.Theinterferencefringesarethenfrozen
atasinglestressstateinthecombinedhologram.Theresolutionisexcellentandcanbedownto
0.2m,Ref.[3433].

34.13.2.3 Moir techniques


TheMoireffectisanopticalphenomenonobtainedwhentwogridsconsistingofparallellineswitha
sufficiently small pitch are superimposed and observed in either transmission or reflection. Any
relative strain disturbance between the two grids produces a diagnostic banding pattern. The
formationofMoirfringesisusedtoevaluaterelativedisplacementsonobjectsurfaces.Thisapproach
ismoreappropriatetostrainmeasurementthandefectdetection.

34.13.2.4 Speckle photography


Alaserbeamilluminatingaroughsurfacegivesrisetoascatteredintensitydistributionwhichtakes
the form of alternately bright and dark spots. This is an interference pattern, known as a field of
speckles. The measurement of the displacements that an object undergoes between two recorded
statesinvolvesopticalfilteringofthedoublerecordedimagestorevealaMoirfringepattern.Thisin
turndepictstheinplanedisplacementcomponent.Ineffect,thenaturalsurfaceirregularitiesareused
inplaceofMoirgridlines.

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AllspecklemethodshavetheadvantageoverMoirtechniquesofnotneedingagridprintedontothe
objectsurface.Electronicspecklepatterninterferometry,ESPI,isbasedonthisprinciple.

34.13.3 Vibration, pressure and thermal loading


34.13.3.1 General
Forholographytowork,physicaldisplacementsareinducedintheobjectbeingtested.Althoughthe
displacements,ineffectstrains,needonlybeverysmall,theobjectcanbelargeorawkwardlyshaped
making direct physical loading inappropriate or difficult. Various solutions have been devised to
producethedesiredeffects.

34.13.3.2 Vibration loading


Vibrational loading can be achieved with a piezoelectric transducer attached to the subject or test
fixture.Ifvibrationalstressingisused,atimeaveragehologramistakenwhilethestructureisexcited.
Arandomexcitationsignalisgenerated,filteredtothedesiredfrequencyrangeandamplifiedtodrive
thetransducer,Ref.[3434].

34.13.3.3 Pressure loading


Theuseofdifferentialpressuresisparticularlyappropriateforsandwichstructureswheretheinternal
cavities can be used to create a temporary straining mechanism, Ref. [3435], [3436]. The pressure
differentialcanbeestablishedbyplacingthecomponentorstructureinavacuumchamber,orinsidea
transparentvacuumbag,Ref.[3437].Inthatthepressureeventuallyequalises,realtimeimagesofthe
fringepatternsarepreferable.
Direct vacuum loading can also be achieved by clamping a vacuum shell onto an area of a larger
surface,Ref.[3435].However,thisthenbecomesacontactNDTtechnique.

34.13.3.4 Thermal loading


Theuseoftransientthermalloadingtoinducesurfacedisplacementscanbeachievedby:

Hotairblowers,Ref.[3438].

Infraredheaters,Ref.[3432],[3433].

Itisusualtoheattheobjectandthentomonitorthecoolingstage.Thismethodcanhighlightdefects
as well as offering information on the thermal distortion of structures under simulated space
conditions,Ref. [3432],[3433].

34.13.4 Electronic imaging


The double exposure of a photographic plate is an accepted means of achieving high accuracy of
recorded displacements. It is however time consuming, costly and operator dependent. This is not
alwaysaproblemfortheexaminationofspacepayloads,suchasreflectors,butitislessattractivein
otherindustrialsectorsdemandingrapidinspection.
The speed of the process can be increased by using a video recording. Holographic images can be
recorded(30frames/second)andanalysedwithouttheneedforfilm.

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Imageplane holograms are produced by a speckle interferometer using a charge coupled device
CCDTV camera, Ref. [3434]. The information can be stored digitally for automated processing and
colourenhancement.Figure34.13.1showsthebasicconfigurationofanelectronicsystem,Ref.[3434].
Electronicimaginghasbeencriticisedfornotofferingthesameimagequalityasconventionaldouble
exposure plate photography. This is likely to change because of rapid progress of computer
enhancementandtheimprovedresolutionofimagingdevices.Nearsurfacedelaminationsof2.5mm
havebeendetected.

Figure34.131Holographybyelectronicimagingwithrandomvibration
excitation

34.13.5 Examination of space structures


34.13.5.1 General
Holographyisnotjustlimitedtodefectanddamagedetection,butcanalsobeappliedtomeasuring
displacementsanddistortions.Someareaswherethishasbeenappliedinclude:

Shearandcompressiontestsofpanelsusingelectronicspecklepatterninterferometry,ESPI.

Thermaldistortionsofantennas,Ref.[3432],[3433].

Vibrationresponseofpanelsandstructures,Ref.[3439].

34.13.5.2 Limitations
Holographic techniques can be disturbed by mechanical vibration which alters the respective
positions of the object and hologram. Consequently the object needs sufficient isolatation
mechanicallytoinhibitsuchmovement.

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Although early holography techniques tended to be time consuming (film technology) and costly,
imagecapture,digitalsignalprocessingandhandlinghaveimprovedgreatly.

34.14

Laser shearography

34.14.1 Introduction
Lasershearographyisanoncontacttechnique,exceptfordirectvacuumloading,thatcanbeapplied
inthelaboratory,inproductionandinservice.
Itisarelativelynewtechnique,whichissimilartoholographyandaimstoprovideameansofrapid,
realtime, largearea inspection. The advent of electronic digital image processing has motivated its
development,Ref.[3440].
Imageshearing speckle pattern interferometry, commonly known as shearography, is a fullfield
laserbased interferometric technique. Shearography measures strain fields on the surface of the
subject, i.e. measurement of outofplane surface displacement (dy/dx) of a body under load.
Measurementsensitivityaslowas0.1straincanbeachieved,Ref.[3441].Shearographybeganasan
electronictechniqueandsoavoidedtheuseofphotographicplates,Ref.[349],[3430],[3440],[3441],
[3442].

34.14.2 Basic technique


34.14.2.1 General
Shearography is a selfreferencing, commonpath, interferometric method, as shown in Figure
34.14.1,Ref.[3440].

Figure34.141Electronicshearographicsystem:Schematicdiagram

Beamsplittingisperformedbytheshearingopticsinsuchawaythatadoubleimageoftheobjectis
formed by the imaging lens (usually a commercial lens) on the CCD sensor. The direction and
magnitudeoftheimageseparation,orshear,isdeterminedbytheorientationoftheshearingoptics.

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Thetwowavefronts,labelledasshearedandunsheared,arecoherentlyaddedintheimageplaneto
produceaspeckleinterferencepatternthatrepresentsauniquespatialsignatureofthetopographyof
the surface of the object. Loading techniques, such as thermal, vibration and vacuum pressure, can
thenbeusedtoinducesurfacedisplacement,Ref.[349].

34.14.2.2 Portable shearography systems


Portablesystemsuseavacuumshellappliedtotheflatorcurvedstructure(e.g.aircraft)toinducea
smallpressuredifferential.Theoperatorholdsavideomonitorandcontrolboxduringthetest,Ref.
[3442].

34.14.3 Characteristics of shearography


Thefeaturesofshearographyinclude:

ItcanoperateinC-scanmode.

Bothportableandfixedscanningsystemsarepossible.

Alignmenttosurfaceisnotcritical.

Itisinfluencedbysurfacereflectance.

Thedetectionresolutionbecomespoorerasthefieldofviewexpands.

Itismoreversatilethanholography,butlessaccurate.

Shearography has been used on assembled structures, such as aircraft, Space Shuttle and Atlas
Centaur.
Table34.14.1givesthetypesofdefectsdetected,Ref.[3442].

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Table34.141Defectdetectionbyshearography
Stressing
Technique

Material

CFRP sheet
Thermal
Honeycomb sandwich
All materials
CFRP sheet

Honeycomb sandwich
Vacuum
Rubber bonded to metal or
composites
Foam core panels
Cork to metal or composites
Vibration

Microwave

34.15

Honeycomb sandwich
Foam to composite or metal
panels
Materials with high dielectric
constant

DefectTypeDetected

Delaminations
Impact damage
Some foreign material
Skin to core debonds
Crushed core
[Thermal expansion]
Impact damage
Delaminations
Porosity
Skin to core and far side
debonds
Sheared core
Crushed core
Debonds
Near surface and deep
debonds
Debonds
Skin to core debonds
Crushed core
Debonds
Entrapped moisture

Thermography

34.15.1 Introduction
Thermographyisanoncontacttechniquethatissuitableforuseinthelaboratory,inproductionand
inservice.
Allthermographytechniquesrelyonthepresenceofadefectdisturbingtheheatflowinacomponent.
Thesurfacethermaldistributionismonitoredbyinfraredcameras.Thedifferentrateatwhichradiant
energyistransmittedordiffusedtothemonitoredsurfaceproducestemperaturevariationswhichcan
indicate the presence of defects. All techniques can now benefit from digital signal processing and
realtime image display. Thermography for detection of defects and discontinuities is principally a
surfaceornearsurfacetechnique.
Thermography is a versatile concept because it is applicable to a wide range of materials and
structures,includingcompositesandmetals.Ithasalsobeenappliedtoceramicmatrixcompositesto
determinetheintegrityofoxidationresistantcoatings,Ref.[3451].Whereverheatflow,conductionor
radiationcanbeinduced,thermographyisapossibleevaluationtool.

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34.15.2 Techniques
34.15.2.1 General
Allthermographictechniquesaimtoestablishheatflowpatternsonthesurfacewhichcanberecorded
andexamined,Ref.[3449];byobservationandmeasurementofthethermaldiffusivityandeffusivity,
Ref.[3443].
Some systems can show the presence of significant impact delaminations over large areas, whilst
othersofferbetterresolutionovermorelimitedareas.Figure34.15.1showsthebasictechnique,Ref.
[3444].

Figure34.151Basicthermographictechnique
34.15.2.2 Real-time video thermography
Thisisageneralclassificationforalltechniquesinwhichcontoursofequaltemperature(isotherms)
are mapped over a surface. The assumption is that defects, inhomogeneities, or other undesirable
conditionsoftheobjectundertestappearaslocalhotorcoldspots.Inspectioncanbeundertaken
from one side, where delaminationtype defects appear as hot spots, or throughtransmission by
viewingthebackfacewherecoldspotsoccur.Inpractice,throughthicknessinspectionisrare.
Surface thermal distributions can be detected by contact or noncontact methods. Contact methods
includethermocouples,temperaturesensitivepaintorliquidcrystals,butthesearelessattractivethan
noncontactmethodswhichrelyuponinfraredradiationtodeterminethetemperaturedistributionof
theradiatingsource.

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Photoneffect devices, sensitive to the infrared wavelengths generated, are used in realtime video
thermographic camera systems that scan the entire surface very rapidly. The wavelength of the
emitted infrared radiation is related to the temperature of the emitting surface through Plancks
radiationlaw.Differentmaterialshavedifferentsurfaceemissivities.

34.15.2.3 Pulsed video or transient thermography


Thisisthemostcommonformofthermographyappliedtocompositestructures,Ref.[3443],[3445],
[3446],[3447],[3448],[3488].Theobjectisheatedbyahighintensitypulseofinfraredlightusually
from a xenon or quartz lamp. This typically produces an increase in surface temperature of about
10C.Theheatflowawayfromthissurfaceisthenmonitoredforabout30seconds,i.e.insinglesided
mode.
Someofthetypicalheatingregimesusedare:

Two 600 mm xenon flash tubes, each delivering 4 kJ over a discharge period of 6 ms giving
typically0.8J/cm,Ref.[3448].

Four xenon flash tubes (rated to 20 kJ total) in a square illuminating 300 mm x 300 mm of
surface(upto2.5J/cm),withpulseof5ms,scanningat5m/min,Ref.[3446],[3447].

Eightxenonlamps,each6kJ,with2mspulseduration,Ref.[3444].

Thermogramimagescanbetakenatintervalsfrom40msto125ms,i.e.from8persecondto25per
second.
The technology has several distinct advantages as an uptodate, noncontact technique. These
include:

Portableandcompact,withitsowndataacquisitionandimageprocessing.

Capable of detecting a wide range of defects in thinsection composite constructions, when


optimised.

Appropriate for different materials (polymers, metals and all composites) for detection of
delaminationsanddisbonds.

Capableofdetectingcorrosionofalloysandwithinbondedmetaljoints,Ref.[3443].

34.15.2.4 Thermal-wave imaging


Thermalwaveimagingtechniquesuseintensitymodulatedheatsourceswithavarietyofdetectorsto
monitordifferencesintheresponseofthematerialtothegeneratedthermalwave.Imagingcontrastis
providedbyvariationsintheresponseofthematerialtothethermalwavegeneration.Theintensity
modulatedheatsourcesaregenerallyeitherlaserbeamsorparticlebeams,thelatterinvacuumonly.
In addition to modulating the intensity of the heat source, e.g. by mechanical chopping of the laser
beam,thelaserisscannedoverthesurface.
Apointbypointimageofthesurfacecanbebuiltupbyelectronicprocessingofthemonitoredsignal.
Thesethermalwavesarehighlydampedandquicklydissipatewithinathermalwavewavelengthor
two.
Dependingonthetypeofdetectingsystemusedtomonitortheresponse,suchtechniquesareusually
describedaseither:

Photooptical, which normally have a second laser beam for the detection of thermalwave
effects;asshowninFigure34.15.2,Ref.[3449].

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Photothermal, which are generally used for large area inspection; as shown in Figure 34.15.3,
Ref.[3449].

Photoacoustic, which monitor pressure pulses established in closed acoustic cells by the
conduction of heatfrom the surface of the examined object in air; as shownin Figure34.15.4,
Ref.[3449].

Thermalwave techniques can be used to assess the quality of adhesive bonds and the integrity of
coatings on metal substrates. The high resolution possible using thermalwave imaging has been
demonstrated by the detection of 10m nearsurface defects in ceramics. It has also been used in a
microscopemodeforimagingmicrostructures.

Figure34.152Thermalwaveimaging:Photoopticaldetection

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Figure34.153Thermalwaveimaging:Photothermalandpiezoelectricdetection

Figure34.154Thermalwaveimaging:Photoacousticgascell

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34.15.2.5 Thermoelastic stress measurement technique


SPATEstresspatternanalysisbythermoelasticemissionusesheatgeneratedfromcyclicloadingasa
meansofobservingdefects,Ref.[3449],[3450].Aninfraredcameramonitorstheradiationemittedat
the maximum and minimum levels of mechanical loading during each cycle. Since the local surface
temperatureisproportionaltotheinstantaneousvolumetricstrain,thetemperaturemeasuredbythe
infrared emission is related to the local principal strains. A raster scan is made from point to point
alongthesurfaceoftheobjecttodevelopanimageoftheprincipalstrainpatternonthesurfaceofthe
objectundertest.
TheSPATE9000systemiscapableofdetectingstresschangesof0.4MPaandtemperaturechangesof
0.001C,Ref.[3450].
It can be a slow inspection method and, because the object is mechanically loaded, is in effect a
contactNDTtechnique.

34.15.2.6 Vibrothermography
This uses mechanical vibrations to setup resonance in damaged areas, leading to locally increased
dissipation of heat. Damage in surface plies is more likely to be detected than subsurface or back
surface damage because of the strong attenuation of heat conducted through the thickness of the
composite.

34.15.3 Heat sources and pulse duration


Early thermographic techniques used hotair guns and quartz halogen lamps. These gave relatively
long heat pulses and proved that it was possible to detect defects such as surface delaminations,
typically 10 mm in size. The steepness of the temperature gradient provides the contrast between
defectiveandnondefectiveareas.Theuseofmorerapidheatpulses,suchasthoseprovidedbyxenon
tubes,improvesthetechnologybyenablingsmallerdefectstobedetected,e.g.about1mmto5mm.
Thisalsoimprovesthescanningrate.
Theprogressiontolaserpulseswithnarrowlyfocusedpointsimprovestheresolutionevenfurther,so
thatsubmillimetresizeddefectscanbedetected.Thisisperhapsmoreappropriateformetals(small
cracks) and metal or ceramic composites (microcracking, porosity and fine delaminations) than the
largerdelaminationsusuallyfoundinpolymercompositeconstructions.
Thethermalconductivityandsurfaceemissivityofthetestmaterialslargelydefinethedesiredpulse
energylevelandduration.

34.15.4 Detection capabilities


AnexerciseconductedbyNNDTC,AEATechnology,UKinconjunctionwithESA/ESTECestablished
thedetectioncapabilitiesoftheTalytherm890transientthermographysystem,Ref.[3448].
A summary of the results of the work with flat bottom holes, FBH, control defects for a variety of
materials is shown in Table 34.15.1, Ref. [3448]. Table 34.15.2 gives the detection limits for FBHs in
mildsteel,aluminiumandcarboncarbonmaterials,Ref.[3448].

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Table34.151Thermography:Summaryofdiameter/depthratiosfromdifferent
studies
Material

Aluminiu
m
Mild Steel
C-C
CFRP
GRP
Delrin

Ratio
(BestExperimental)

Ratio(Best
Quoted)

Numberof
DataPoints

RangeofDepth
ofDataPoints

0.4 for d = 5.0 mm


2.0 for d = 2.0 mm
2.0 for d = 3.2 mm
2.1 for d = 3.0 mm
1.6 for d = 7.0 mm
9.1 for d = 2.2 mm

0.5
1.5
4.0
1.8
-

6
5
3
10
2
4

1.0 - 5.0 mm
1.0 - 2.0 mm
1.0 - 3.2 mm
1.0 - 3.0 mm
5.0 - 7.0 mm
1.0 - 2.2 mm

Key:d=depth

Table34.152Thermography:Detectionlevelsestablishedforflatbottomedholes
(FBH)fromESTECstudy
DepthofFBH
(mm)

Min.Diameter
Detectable(mm)

Diameter/
DepthRatio

PulseRequired
(kJ)

Temperature
Window(C)

1, 2 or 4
4
4

4, 6, 15
4, 6
4

1, 2 or 4
1, 2 or 4
2 or 4

4, 6, 15
4, 6, 15
4, 6

4
4
4
4

4, 6
4
4
4

MildSteel

0.5
1.0
2.0

2.0
2.0
4.0

4.0
2.0
2.0
Aluminium

0.5
1.0
2.0

4.0
4.0
8.0

8.0
4.0
4.0
CarbonCarbon

1.0
2.0
3.0
4.0

4.0
4.0
6.0
6.0

4.0
2.0
2.0
1.5

34.15.5 Limitations of thermography


The limitations of thermography usually show themselves when the defects do not lie near the
inspection surface. Throughthickness inspection is rarely feasible, and this is creates particular
difficultieswhensandwichconstructionsareinspectedfordefectsadjacenttothebackfaceskin,e.g.
skintocoredisbonds.
Themanufactureofrepresentativedefectsincompositepanelsposesproblemswhenthermography
systems are optimised or calibrated. For ultrasonics, defects such as interlaminar debonding can be
simulatedbyincludingareasofplasticfilm.Thermographictechniquesdetectthelargedifferencesin
thelocalthermalconductivitybetweenthecompositeanditsdefects.Suchdefectsaregenerallythin

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airgaps(delaminations)whichhaveverypoorthermalconductivity,whereasasolidinclusion,such
as plastic film, does not respond in an acceptable manner because the local thermal conductivity
remainsfairlyhigh.Forthisreason,flatbottomedholes,FBH,drilledfromthebackfaceareusedto
establishthedetectioncapabilitiesofthermographyfordifferentmaterials.Detectionlevelsarethen
defined by a diameter to depth ratio; where diameter is the hole diameter and depth is the
maximum subsurface distance from the inspection face at which the bottom of the hole can be
detected,Ref.[3443].

When a comparison is made of the results from different studies over a period of 10 years, a
considerabledegreeofscatterisevidentintheclaimsfordetectionlevels,ratiosofdiameter/depth,in
differentmaterials,Ref.[3448].Inconsistenciescanbeattributedtovariationsinmaterials,heatpulse
energyordurationandtheefficiencyofdetectionsystems.
Thermography is continually improving, but a point has been reached where the best techniques
availableneedtobeevaluatedunderrepresentativeconditionstodefinetheirtruecapabilities.

34.16

X-ray radiography

34.16.1 Introduction
34.16.1.1 General
Xrayradiographyisnoncontact,exceptwhenusingcontrastenhancingmedia,andcanbeappliedin
thelaboratory,inproductionandinservice.Itisalongestablishedmeansofinspectingcomponents
and structures. Traditionally, the image was recorded on photographic film, giving high resolution
and good contrast, but was rather time consuming. Film is being replaced by electronic imaging,
enablingrealtimeviewingandimagemanipulationorprocessing.

34.16.1.2 Advantages of radiography


TheadvantagesoffilmXrayradiographyinclude:

The ability to image the internal structure and defects within a subject, be it a laminate,
sandwichpanelorassembledstructure.

Differentiationofmaterialphaseswithdifferingdensitiesorthicknesses.

Cleardetectionofthepresenceandorientationofindividualcomponents,e.g.honeycombcore,
pottingcompound,fastenersandsolidcontaminantsorforeignbodies.

Reasonable detection of resin enrichment, porosity, prepreg gaps, fibre alignment and layup
orderincomposites.

ForCFRPcomposites,lowXraytubevoltages(eV)needtobeused,duetothelowatomicnumbersof
carbonandhydrocarbonmatrices,i.e.theyhavealowXraystoppingability.

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34.16.1.3 Limitations
ThelimitationsoffilmXradiographyonpolymercompositesinclude:

FilmXraysprovideatwodimensionalimage(shadowgraph)throughthesubject,thereforethe
presenceofananomalycanbedetectedbutthelocationwithrespecttodepthisunknown.

Xrayscannotdetectdisbonds,delaminationsandairgapswhenthesedefectsarenormaltothe
irradiationdirection,e.g.wheninspectingmostlaminatesandsandwichpanels.Theamountof
contrastproducedbyanyneartwodimensionaldefectishighlydependantuponitsorientation
withrespecttotheXraybeam.

FilmXraysaretimeconsuming,bothinexposureandfilmprocessing,andcannotprovidereal
timeimaging.Thereforetheyaredeemedcostlyformanyapplications.

The advent of digital radiography and computer tomography go some way to overcoming these
limitations,[See:34.17].
Theuseofcontrastenhancingmedia,suchastetrabromoethane,TBE,forthedetectionofnearsurface
defects,e.g.cracksanddelaminations,isconsideredrelevantfortestpurposesonly.Penetrationofthe
laminate is needed, albeit small, to enable entry of TBE. This contaminates the composite and the
inspectionbecomesacontactprocess.

34.16.2 X-ray techniques


34.16.2.1 General
TherearevariouswaysinwhichXradiographycanbeundertaken,including:

Basicradiography,

Microfocus,

Backscattering,

ScatteringAndRefraction,

backscattering.

34.16.2.2 Basic radiography


This is the traditional technique where variations in radiation absorption by different constituents
producedashadowimagethroughthesubjectmaterialorcomponent.
Excellentcontrastcanbeachievedbetweenthefeatureswithintheobject,providedthatthediverging
Xraybeamiscontrolledcorrectly.Theimagecharacteristicsaredeterminedbythe:

Materialdensity,

Materialthickness,

Appliedelectronvoltage(XraytubeeV),and

Exposuretime.

It is a powerful tool for nondestructive testing of metal, polymer composite and multimaterial
structures.

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34.16.2.3 X-ray microfocus


ThisissimilartoconventionalXrayinspection,butaverynarrowbeamofXraysisusedtoexamine
thelocalmicrostructureofmaterials.Thetechniquecanresolveverysmalldefects.Someapplications
aretheexaminationofcarboncarbonandCMC.

34.16.2.4 Backscattering
ThisreliesontheComptoneffect.AfinelycollimatedbeamofXraysisdirectedthroughamaterialat
anobliqueangletothesurface.Someofthephotonsarescatteredbackthroughthesurface.Afinely
collimateddetectorcanthenbeusedtomeasuretheradiationwhichiscomingfromasmallvolumeof
materialattheintersectionoftransmittedandscatteredradiationpaths,Ref.[3452].Thisisineffecta
singlesidedmethod,withaccesstothebackfacenotrequired.
Thebackscatteringtechniquehasbeenusedforthicknessanddensitymeasurementofcarboncarbon
materials,Ref.[3452].Cscanimagescanalsobeconstructed.

34.16.2.5 X-ray scattering and refraction


VariousmodificationstotraditionalXrayinspectionareappearing,basedonscatteringandrefraction
behaviours,including:

Scanningdiffractometry,Ref.[3453].

Scanningtopometry,Ref.[3453].

Diffractionscanningmicroscopy,Ref.[3453].

Xrayrefractometry,Ref.[3453],[3454].

34.16.2.6 - backscattering
ThisisasimilartechniquetoXrayscattering,butusingelectrons.

34.16.3 Digital radiographic system developments


34.16.3.1 General
TheadventoflowcostcomputingpowerandchargecoupleddeviceCCDcamerashasenabledfilm
photography to be superseded by digital systems, Ref. [3455]. The quality of the viewable Xray
imagedependsontheradiographicequipmentanddigitaldatasystem.
ThemajorXraysystemsincurrentuseareshowninFigure34.16.1,Ref.[3455].Eachsystemprovides
differentimagingcharacteristics.

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Figure34.161Typicaldigitalradiographysystems

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34.16.3.2 X-ray image intensifier


Thisiswidelyfoundinmedicalandindustrialapplications.Typicalvacuumtubesystemsobtaintheir
gainvalue(x30tox10000)bytheuseofaninputXraytolightphosphorscreenthatconvertsXray
imagingphotonsintolightphotons.Thelightphotonsarecapturedbyaphotocathodeandconverted
to electrons. These are accelerated to many thousand eV and are electrostatically focused onto an
outputphosphor.Heretheelectronsareconvertedbackintolightphotonstoprovideanopticalimage
corresponding to the impinging Xrays. A lens is then attached to this output phosphor, and a
television cameraisused to collect the optical image. Theintensificationis not solely electronic, but
canincludeareductioninarea;wherebytheelectronsfromalargeareainputscreenarefocusedona
smalloutputscreen.

34.16.3.3 X-ray phosphor/camera system


In some cases image intensification is not necessary, which provides more flexibility. The Xray
phosphorcanberemovedfromthevacuumtubeanduseddirectlyonorshapedovertheobject.The
glass window that absorbs much of the low Xray energy imaging photons is no longer needed, so
highercontrastimagescanbeobtained.Animageisoconcameraistypicallyusedinthissystem.

34.16.3.4 Linear array scanner


AfannedXraybeamisscannedacrosstheobject,andtheemergingXraysarecollectedbyalinear
arraydetector.Thecollecteddataisbuiltupintoanimagebyacomputer.Thedisadvantagesofthis
systemincludethe:

Longimageacquisitiontimes,

LowXraybeamutilisationefficiency,resultinginhighXraytubeloading.

In most systems the detector consists of an Xray phosphor in direct contact with a semiconductor
photodiodearray.Thecrystalsaredicedintothick,highlyXrayabsorbingpiecesandbecomediscrete
pixelsinthesystem.
An advantage of linear array systems is that a collimated fan beam and detection system has
significantlyreducedXrayscattercomparedwithnoncollimatedbeams,soproducingveryaccurate
images;henceitsuseinCTcomputerisedtomographysystems.

34.16.3.5 Fibre optic CCD system


FurtherdevelopmentsofXrayphosphortechnologyandCCDqualityhaveprovidedanopportunity
tocustomdesignanXrayinspectionsystem;suchastheFOSCCDcamera,Ref.[3456].
A fibreoptic scintillator is in many ways equivalent to a fibreoptic faceplate window except that
luminescentglassfibresareusedasthecorematerial.Corediametersinthesefaceplatesareusually
between10mand20m.WhenexposedtoXrays,scintillationwithineachcoreischannelledtothe
faceoftheplate.ThisprovidesaverysharpimageplanethatcanbedirectlybondedtoaCCDarray.
TheFOS/CCDsystemoffershighXrayabsorption,improvedimageacquisitiontimeandXraybeam
utilisation over the linear array because the FOS can be made thick for high Xray absorption
efficiency. As the CCD is a solidstate device, it is not prone to geometric distortions and shading
problems that are inherent in tube systems. As CCD chips become larger and contain higher pixel
densities,fieldofviewlimitationsoftheFOS/CCDsystembecomelessimportant.AFOS/CCDsystem
is lightweight and rugged and can easily be built into a scanning system for inspection of large
aerospaceassemblies.

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34.16.4 Defect resolution


Like ultrasonics, Xray techniques are evolving to make them more appropriate to inspection
activities.Themaindevelopmentscentreon:

Singlesidedinspectionusingbackscatteringtechniques,asneededforassembledstructures.

Highresolutionmethodsforceramicmatrixandcarboncarboncomposites,andforindividual
components.

34.17

Computer tomography

34.17.1 Introduction
Computertomographyisanoncontactmethodthatcanbeusedinthelaboratoryandinproduction.
ThreedimensionalXrayimagingispossibleusingcomputeraidedtomography,CAT,whichbuilds
upsuccessivecrosssectionsofthecomponent,Ref.[3410],[3457].Thismethodisalsodescribedas
computertomography,CT.
Initially a medical technique, it has been used to examine highvalue or critical items with complex
materials and geometries. The equipment is large, nonportable and expensive, but can produce
excellent results with components otherwise difficult to inspect reliably. It is also applicable to
structurescontainingavarietyofmaterialtypes,e.g.:

Metalmatrixcomposites,Ref.[3456],

Ceramicbasedmaterials,Ref.[3458],

Rocketmotorormissileparts,

Turbineblades,and

Highlycontouredcarbonfibrebasedcompositecomponents.

34.17.2 Basic technique


A thin slice of radiation is passed through an object and the transmitted intensity is measured by a
detector array, Ref. [3459]. The radiation levels are typically from 10 keV to 40 keV for lowenergy
radiationorfrom80keVto120keVforhighenergy,Ref.[3457].
Theobjectisrotatedinordertoprovideviewsfrommanydirections.Thedataisthenprocessedby
computer to derive a twodimensional Xray attenuation map of the slice, corresponding to volume
elementswithintheinterioroftheobject.Ifmultipleslicesaretakenovertheentirepart,acomplete
threedimensionalreconstructioncanbemade.Thecomputerenablesthisthreedimensionalmapto
beexaminedinanumberofways(spatialanalysis).ACTfacilityisshowninFigure34.17.1,Ref.[34
60].

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Figure34.171Computertomographyfacility
The 2D and 3Dimage reconstruction overcome two of the main deficiencies of conventional
radiographybydefiningthelocation(depth)ofadefectandvisualisingdefectsnearnormaltotheX
rays,asinplanardelaminations,Ref.[3461].
CT can be applied to quality acceptance inspection, product development and failure analysis. It
providesaccuratequantitativedataonmaterialdensitydistribution,presenceofconstituentpartsand
dimensions.

34.17.3 Attributes of CT scanning


34.17.3.1 General
TheprincipalattributeofCTisthedetailedinternalexaminationofdiscrete,complexassembliesand
subcomponents.Somepracticalexamplesofthisinclude:

Compositesandwichwingleadingedgesandairfoilsections,Ref.[3456],[3460],[3462].

Pottedtransformers,Ref.[3459].

CFRPJandZstiffeners,Ref.[3460].

BondedTspars,Ref.[3462].

Metalcastings,Ref.[3459].

Titaniumcomponentsmadebysuperplasticforminganddiffusionbonding(SPF-DB),Ref.[34
63].

Helicopterrotorblades,Ref.[3464].

AnindicationofthequantitativeaccuracyofCTscanningcanbestatedas:

Measurementofmaterialdensityvariationsintherange0.1%to1.0%,Ref.[3463].

Typical measurement accuracy in the range 0.05 mm to 0.25 mm (50 m to 250 m), for
components0.05mto0.5minsize.

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The availability of a technique which can conduct nondestructive sectioning of complex


components, as opposed to the alternative destructive examination has important implications in
productdevelopment,Ref.[3459].
Reduced development time can result in significant initial cost savings and a reduced risk of poor
designsbeingmanufactured.Thiscanresultinlargesavingsoverthelifetimeofaprogramme.
The ability to detect volumetric defects by a noninvasive inspection technique enables a range of
defectstobedetected,includingthoseofprimaryconcernincomposites,i.e.:

Delaminations,

Coretoskindisbonds,

Misplacedmaterials,and

Foreignbodies

34.17.3.2 Limitations
ThefundamentallimitationsofCTare:

Expensiveequipment.

Notportable.

Limitationofcomponentsize;usuallylessthan1m,buttypically500mm.

Facilities for inspecting large structures, up to 1.8 m and eventually 3.8 m in diameter have been
reported.Theseareintendedtobeusedfortheinspectionofsolidrocketmotors,Ref.[3465].

34.17.4 Micro-tomography
With the right equipment, CT can be applied to the examination of material microstructures with
spatialresolutiondownto20m;termednoninvasivemicroscopy,Ref.[3463],[3466].Thepixelsize
setbythedetectordeterminesthelevelofresolutionwhichcanbeachieved.
Thistechniquecanbeusefulforexaminingcomplexmaterialssuchasceramicmatrixcomposites,Ref.
[3458],orassembliesforreusablespacevehicles,suchasCSiCairintakeramps.

34.18

Eddy currents

34.18.1 Introduction
Eddycurrenttechniquescanbeclassedaseithercontact(byhand)ornoncontact,whenautomated
scanningisused.Itcanbeappliedinthelaboratory,inproductionandinservice.

Inthistechniquecurrentlooppaths,eddycurrents,areinducedinaconductivematerial,bypassing
analternatingcurrentthroughacoilcontainingprobe,Ref.[3467].Theprobeisplacedonornearthe
conductivesurfaceofthecomponent.Defectsaredetectedbymonitoringdisturbancesintheinduced
magneticfields.

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Itisprimarilyusedforconductivity,crackandcorrosiondetectioninmetals,andiswidelyusedfor
manualorautomatedaircraftinspection,Ref.[3469].Eddycurrenttechniquesformetalsworkinthe
10 kHz to 1 MHz range. It is particularly appropriate for examining bolt and rivet holes to locate
cracks.

Sufficient electrical conductivity for eddy currents to be induced can also be found in CFRP (> 40%
volume fibre), carboncarbon, Ref. [3470], CSiC and metal matrix composites. Practical inspection
systemsarethereforefeasible,Ref.[3410].Automatedinspectionhasbeencarriedoutofsolidrocket
motor casings, forgings and segments, Ref. [3468], in conjunction with electromagnetic acoustic
transducers(EMAT).

34.18.2 Developments in eddy current techniques


34.18.2.1 General
Computerised eddy current scanning systems are suitable for the inspection of composite
constructions.SomeobservationsconcerningeddycurrentsasappliedtoCFRPare,Ref.[3471]:

Highfrequenciesareneeded,Ref.[3472],e.g.:

10MHzto500MHzforUDCFRP,and

1MHzto30MHzforwovenCFRPlaminates.

Eddycurrentsareaffectedbylaminateedges,soperipheraldefectscanbedifficulttoresolve.

Coilprobedesignisinimportantinrelationtothelaminateconstruction.Thenumberofcoils,
their shape (horseshoe, pancake elliptical) and width should be optimised in relation to the
laminatethickness,Ref.[3470],[3472].

EddycurrentprobescanbeoperatedtoproduceCscanimages.

Inducededdycurrentstendtobeconcentratednearthesurfaceofthematerialadjacenttothe
coil, although some control of the penetration depth can be achieved by varying the
characteristicsoftheappliedsignal.

Eddycurrenttechniqueslookpromisingforthelocatingof:

Brokencarbonfibres.

Changesincarbonfibrevolumefraction.

Changesincarbonfibrelayupandorientation,Ref.[3410].

Detectingdisbondsbetweenmetalsheetandcompositelaminate,Ref.[3473].

34.18.2.2 Limitations
Delaminationsaredifficulttodetectunlesstheinterlaminardamageisfairlysevere(plyseparation).
Thedetectionofdelaminationsisimprovedif:

Morethan20%ofinterfacialplycontactislost,or

Fibreshavebeenbroken,toatleast8%ofthethickness,Ref.[3472].

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Table 34.18.1 gives the results of a test programme to compare the detection capability of an eddy
currenttechniquewiththatofultrasonics,Ref.[3472].

Table34.181Detectionofdamagebyeddycurrentandultrasonics
Construction

ImpactEnergy
(J)

Sandwich:
0.5 mm
skins
6.8 mm core
Sandwich:
2.0 mm
skins
6.8 mm core
Laminate:
7.2 mm
CFRP

0.69
1.33
2.39
2.83
5.59
9.12
17.5
5.72
10.7
27.3
37.5
41.7

EddyCurrent
Image

UltrasonicImage
SpotDiameter
(mm)

Visible
Damage

Not visible
Halo
Halo

11 - 15
16 - 20
20 - 26

Not visible
Dent, BF
Hole

BV halo
Halo
Halo
Halo
Not visible
BV dark spot
Dark spot,
halo
Halo
Light spot

18 - 22
37
33
41
15
22
29
33
41

Not visible
Dent
Dent
Hole
BV dent
Dent, CM
Dent, CM
Dent, CM
Dent, CM

Key:

SkinswovenCFRP;Corealuminium.

BVBarelyvisible;BFBrokenfibres;CMCrackedmatrix.

34.18.2.3 Future developments


Some of the developments that increase the relevance of eddy current testing to both metals and
compositesinclude:

Scanningsystemsforassembledstructureswithmultiplematerials.

ImproveddefectdetectionforCFRPandcarboncarbon.

Conditionmonitoringofalloystructuresandfasteners.

34.19

Other NDT techniques

34.19.1 General
There are other techniques which can be used for inspection, but they are not common and tend to
havespecialisedroles.Thetechniquesdescribedare:

Microwave

Heat and photosensitive agents

Electrical impedance

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Acoustic microscopy

Nuclear magnetic resonance(NMR)

Neutron radiography

Gamma radiography

D sight - Diffracto sight

34.19.2 Microwave
Microwavetechniquesarenoncontactandcanbeappliedinthelaboratoryandinproduction.
Any disruption in microwave throughtransmission in composites indicates the presence of
discontinuities, or variations in dielectric material properties, Ref. [3410]. Changes in amplitude or
phasecanbeobserved,enablingthedetectionofdefects,thicknessanddegreeofresincure.
Thetechniquehasbeenappliedtofilamentwoundstructures,andalsoforsinglesidedexamination
ofsandwichpanels,Ref.[3474].Typicaldefects,suchasdelaminationsandskintocoredisbonds,can
bedetectedwhentheequipmentisscannedoverthesurfaceandoperatedintheXbandrangewith
frequenciesbetween8.2GHzand12.4Hzandat24GHz.

34.19.3 Heat and photosensitive agents


Techniquesusingthermochromicandphotochromicsubstancesarecontactmethodsandsuitablefor
useinthelaboratoryandinservice.
Thermochromic and photochromic substances show changes in colour or light characteristics
depending on their exposure time and temperature history. They can be applied to surfaces of
componentsaspaints,partofacrackdetectionsystemorcombinedwiththeresinmatrix.

34.19.4 Electrical impedance


Impedancetechniquesarecontactmethodssuitableforuseinthelaboratory.
For CFRP materials, electrical impedance measurements can provide a means of indicating the
presence of delaminations, microcracks and moisture absorption, Ref. [3476]. Initial work involved
the immersion of the composite in an electrolyte, so it has not yet been demonstrated as a practical
inspectionmethod.

34.19.5 Acoustic microscopy


These techniques are contact methods, suitable for use in the laboratory or in production. They are
principallyusedforachievinghighresolutionimagingofsmallareas.Thevarioustechniquesare,Ref.
[3476]:

Scanning laser acoustic microscope (SLAM), which provides realtime images in transmission
modethroughoutthethicknessoftheobject.

Scanning acoustic microscope (SAM), which provides highresolution images of surface and
nearsurfacewhenrasterscannedandoperatedinreflectionmode.

CSAM,a variant of SAM, which provides goodormoderate penetration inpulseecho mode


andimagesataspecificdepth.

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These techniques are only appropriate to polymer composite structures under exceptional
circumstances,butaremorelikelytobeofvalueforceramicmatrixcomposites.

34.19.6 Nuclear magnetic resonance (NMR)


NMRisanoncontactmethodthatcanbeappliedinthelaboratoryandinproduction.
It is ananalytical technique commonlyused toassess the chemistry of materials.However,in some
specificcircumstancesNMRcanbeappliedtomaterialsproblems,suchas:

Detectionofmoistureincomposites.

Curingandthicknessofadhesivebonds.

Assessmentoftheadhesivelinerbetweenpropellantandinsulatorinsolidrocketmotors,Ref.
[3477].

34.19.7 Neutron radiography


Neutronradiographyisanoncontactmethodsuitableforuseinthelaboratoryandinproduction.It
issimilartotheXraytechnique.
Imagesareformedonfilmbyneutronsfromaradiationsource.Certainelementsshowhighneutron
absorption, such as boron, hydrogen, lithium and cadmium, whilst others are virtually transparent.
Applicationexamplesinclude:

Composites:

fibrealignment,

moisture,

resinoradhesivebuildup.

Bondedjoints:

bondlinecorrosion.

Neutron radiation computer tomography can also be undertaken on gas turbine engine blades and
aluminiumforgings,Ref.[3478].

34.19.8 Gamma radiography


Usingaradioactivesource,thegammarayspassthroughthesampleandaredetectedonfilmorby
meters.Changesintheabsorptioncharacteristicsbecauseofdefects,densityorthicknessvariationsin
compositesaredetectable.

34.19.9 D sight - Diffracto sight


Thisisanoncontactmethodsuitableforuseinthelaboratory,inproductionandinservice.
Dsightisanopticaltechnologyinthevisiblespectrum,Ref.[3479],[3480].ItusesaCCDcamera,a
whitelightsourcemountedslightlybelowthecameralens,andaretroreflectivescreen.Thesurface
to be inspected is positioned between the cameralight and the retroreflective screen, as shown in
Figure34.19.1,Ref.[3479].

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Figure34.191DsightDiffractosightschematic
TheretroreflectivescreenisthecriticalopticalelementinDsight.Itreturnslightfallingonitssurface
efficientlybackalongtheincidentdirection;unlikeamirrororaprojectionscreen.Thelightreturned
by the retroreflector is slightly dispersed owing to the physical and optical characteristics of the
microbeadsmakingupthescreensurface,butmostofthelightreturnswithina1cone.
Whenthesurfacetobeinspectedisilluminatedbythelightsourceatalowgrazingangle,anylocal
curvaturevariationsonthissurfaceactasafocusordispersethelightontotheretroreflectivescreen.
Adistinctpatternoflightintensitiesthendescribestheviewedsurfaceandhighlightsanyanomalies,
suchasthoseassociatedwithimpactdamageandnearsurfacedelaminations.
Thetechniquehasbeendevelopedforinspectingaircraftandislimitedtodetectingsurfaceandnear
surfacedamage.

34.20

NDT for adhesive bond defects

34.20.1 General
Themainclassesofdefectthatoccurinadhesivejointsare,Ref.[3481]:

Completedisbonds,voidsorporosityintheadhesivelayer.

Pooradhesion,i.e.aweakinterfacebetweentheadhesivelayerandoneorbothadherends.

Poorcohesion,i.e.aweakadhesivelayer.

34.20.2 Disbonds, voids and porosity


Somedisbondsareessentiallylarge,flatvoidsthatcanbecausedbyacompletelackofadhesiveorby
the adhesive being applied unevenly to one adherend only. Disbonds can also be caused by the
presenceofgreaseorothercontaminantsonanadherend,e.g.releaseagent.Inthesecasesthesurfaces
of the defect are generally in close proximity or touching, which makes their detection difficult.
Disbondscanalsooccurasaresultofimpactorenvironmentaldegradationaftermanufacture.
Porosity is caused by volatiles or air trapped in the adhesive. Inadequate drying of composites can
cause absorbed moisture to vaporise during the adhesive cure cycle and produce bubbles in the
adhesive.

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Suchdefectscanseriouslyimpairbondperformancebutcanbedetectedby:

Conventionalwatercoupledultrasonics:Sensitivetodisbonds,delaminationsandporosity.

Ultrasonicbondtesters:Fordisbondsanddelaminations,butnotporosity:

100kHzto1MHz.

Bondascope,whichmeasuresmagnitudeandphaseoftheultrasonicimpedance.

Fokker bond tester II, using a spectroscopic approach monitoring frequency and
amplitudechangesinthefirsttwomodesofthroughthicknessvibration.

Sonicvibrationandmechanicalimpedance:Forlargedefects.

Thermography,Ref.[3415],[3445],[3484],holographyandshearography:Forthelargernear
surface,airgapdefects.

Eddycurrents:Possiblefordisbondsbetweencompositeandmetal,Ref.[3485].

34.20.3 Cohesion and adhesion


A weak adhesive layer, giving poor cohesive properties, can result from incorrect mixing or
formulation of twopart adhesives, or inadequate curing. Since onepart film adhesives also suffer
fromtheseproblems,miscuringseemsthemostlikelycause.Thereissomeevidencetosuggestthat
theFokkerbondtesterMkIIcandetectpoorcohesionundersomecircumstances.
Pooradhesionislikelytobecausedbysurfacecontaminationorincorrectsurfacepreparationpriorto
bonding. A further possibility is contamination by release agent on peel plies. High resolution is
needed within a thin layer of about 1 m thick, which implies the use of ultrasonics at high
frequencies(20MHzto200MHz).Thisleadstoseveresignalattenuationproblems.
Theinspectionofadhesivebondsforpoorcohesionoradhesionremainsanareaofweaknesswithin
NDT techniques, and no reliable method exists currently. As the desire to detect these anomalies
continues, it remains a motivation for new developments, Ref. [3482], [3483]. Until a technique is
proven, adhesion and cohesion problems are best eliminated by precise process monitoring, with
controltestsamplesmadealongsideproductionitems.

34.21

NDT for space applications

34.21.1 Introduction
The number of NDT techniques available has increased considerably within 20 years. They are still
evolvingintheareasof:

Noncontactinspection.

Digitalsignalmanipulationandimagepresentation.

Automationforrapidinspectionandrealtimeimaging.

Itiswidelyacceptedthatmorethanonetechniqueisusuallynecessarytodetectallpossibledefectsor
anomalies that can occur in composite constructions. However, critical defect types are usually

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identifiedforaparticulardesignandmethodofconstructionandthisenablesNDTtechniquestobe
selectedbytheirdetectioncapabilities.
Thedetectionofgrossdefectsremainsamainrequirementfordamagetolerantdesigns.Suchdefects
canbeclassifiedasmissingormisalignedmaterial,delaminations,disbondsandimpactdamage.
Conventional Cscan ultrasonics and Xray examination remain the most powerful techniques for
comprehensivedefectandanomalydetection.

34.21.2 Developments in inspection


The development of inspection techniques has gone beyond the stage of providing a means of
detecting defects in specific materials, such as CFRP. Techniques should be adaptable in order to
inspect a range of materials, complex subassemblies and integrated structures. Some examples of
developmentsthatareaimedatassistinginspectionwithinspaceprogrammesinclude:

Sandwichconstructionsbynoncontacttechniques,Ref.[3421],[3427],[3430],[3432],[3433],
[3474].

Assembled structures by noncontact techniques, Ref. [349], [3412], [3415], [3416], [3437],
[3441],[3443],[3447],[3464],[3469],[3479],[3480],[3488].

Detection of impact delaminations in polymer composites, Ref. [348], [3438], [3446], [3461],
[3475],[3476].

Integrityofadhesivebonds,Ref.[3445],[3481],[3482],[3483],[3484],[3485].

Rocketmotorcasings,Ref.[3465],[3468],[3477].

Integritycontrolofhightemperaturestructures,Ref.[3490].

Aircoupledultrasonicinspection,Ref.[3421].

Microstructuralexaminationofceramiccomposites,Ref.[3419],[3451],[3459],[3490].

Coated carboncarbon components by eddy currents, ultrasonics, thermography and


backscattering,Ref.[3452],[3486].

NDEoftitaniumMMCringsbyultrasonicsandcomputertomography,Ref.[3487].

[See:Chapter76forintegritycontrolaspectsofhightemperaturestructures]

34.21.3 Summary of NDT techniques


Table 34.21.1 gives a summary of the relevance of the main NDT technologies to the inspection of
polymercompositestructures.

[See:Chapter80forNDTofmetalandceramicbasedmaterialsandassemblies]

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Table34.211SummaryofNDTtechniquesforpolymercompositespace
structures
Technique

Comments

Conventional C-scan Good all-round capabilities.


ultrasonics
Good for flat or curved composite panels and sandwich
[C]
constructions.
Good all round capabilities.
X-ray techniques
Good for components, sandwich constructions and
[NC]
assembled structures.
Holography
Good capabilities for inspecting assembled structures.
[NC]
Applicable to sandwich constructions, e.g. antennas.
Acoustic Emission
Of very restricted use, e.g. to pressure vessels during
[C]
proof loadings.
Requires further development.
Laser Ultrasonics
Possible detection of surface or near-surface defects,
[NC]
e.g. delaminations and disbands.
Applicable to rapid inspection of assembled structures.
Probable detection of surface or near-surface defects,
Laser Shearography
e.g. delaminations and disbonds.
[NC]
Applicable to rapid inspection of assembled structures.
Probable detection of surface or near-surface defects,
Thermography
e.g. delaminations and disbonds.
[NC]
Applicable to rapid inspection of assembled structures.
Computer
Good capabilities for defect detection in discrete
Tomography
components or subassemblies, e.g. CMC and C-C.
[NC]
Requires further development for application to CFRP
and C-C.
Eddy Currents
Established technique for inspecting metal
[C or NC]
constructions.
Applicable to inspection of assembled structures.
Key:[C]contactmethod;

[NC]noncontactmethod.

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34.22

Rupture tests

34.22.1 Application
34.22.1.1 General
Sincemanyloadcaseshavelowmarginsofsafety,itisnotpossibletoperformrupturetestsunderall
circumstances.

34.22.1.2 Envelope load case


Anenvelopeloadcaseisdefinedandthetestisconducteduptorupture,where:

Theenvelopeshouldbedefinedatanearlystageoftheproject

Thisenvelopeloadbecomesadimensioningloadcase,whichcanleadtomasspenalties

Theinteractionbetweenloadsisnotwellknownnearrupture

34.22.1.3 Single load cases


Asingleloadcase(theonewhichhaseitherlowestmarginofsafetyorhighestdegreeofuncertainty
ofanalysis)isdefinedforrupture,where:

Itdoesnotgivetherealmarginsofsafetyofthestructure.

Thetestisdoneattheendofthetestsequencebutthestructurebecomesunavailableforfurther
eventualtests.

34.22.1.4 No rupture test


When a no rupture test is done, it should be selected at project level, since the selection takes into
account:

Massbudgets,

Degreeofsafety,

Degreeofabilitytocarryhigherloads,

Costeffects(numberofqualificationspecimens).

For composite structures, rupture often occurs suddenly because no plasticity exists. Hence, it is
difficult to know from a test how far the structure is from rupture. To improve the situation, the
structureisinstrumentwith:

Straingauges(many)tocorrelatemodels.Theoutputenablesreferencetodevelopmentrupture
testsonsmallerparts.

Acousticemissiondeviceswhichcanindicateoftheinternalstateofdamage.

34.22.1.5 Displacement measurement


Tomeasuredisplacementsunderload,techniquessuchasholography,Ref.[3433],shearographyand
EPSIelectronicspecklepatterninterferometryareapplicable.

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34.23

Test related items

34.23.1 General
Anoverviewoftestrelateditemsispresented,whichdescribestheinfluenceofeachitemofthetest
andtheirrelationshiptoeachother.

34.23.2 Major items


Themainitemsthatcanbeidentifiedare:

Failuremodesofthestructureoranypartofthestructure,e.g.:

matrixcracking,

ruptureoffibres,

buckling.

Controlsatanyphaseofthetestofthestructureoranypartofthestructure,e.g.:

deformationmeasurement,

visualinspection,

acousticemission.

Relevantareasofthestructure,e.g.:

locallyloadedareas,

stiffeneredges,

holes.

Typeofloadsthestructurecanpossiblyexperienceduringitslifeorduringtests,e.g.:

static,

dynamic,

acoustic,

impactloads.

Typeoftestsappliedduringallphasesoftheproduct,e.g.:

development,

qualificationtest.

TheinterrelationshipbetweentheseitemsisshowninTable34.23.1.

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Table34.231Interrelationshipofitemsinfluencingthetest

Failure
Modes
Controls
Areas
Loads
Tests

Failure
Modes

Controls

Areas

Loads

Tests

X
X
X
X

O
X
O
O

X
O
X
X

O
X
X
X

O
X
X
O

0:Notapplicable

34.23.3 Qualification tests


34.23.3.1 General guidelines
Somegeneralguidelinesforqualifiedtestingaregiven.Theinterrelationshipoftheeffectsisindicated
inthetablescited.

Effectsoflocalmodeoffailureontheglobalbehaviourofthestructureareassessed;asgivenin
Table 34.23.2.

Testinstrumentationenablesthedetectionofanymodeoffailureduringtests;asgiveninTable
34.23.3.

Localanalysisliststhepossiblemodesoffailureforeachareaofthestructure.Criticalpointsare
studiedduringtests;asgiveninTable34.23.4.

Effectsofeachtypeofloadsaswellascombinationsareassessed;associatedmodesoffailure
arelisted;asgiveninTable34.23.5.

Effectofeachmodeoffailureareanalysedthroughtheappropriatestagesduringthelifeofthe
project;asgiveninTable 34.23.6.

Each particular area of the structure is instrumented with respect to its probable mode of
failure;asgiveninTable34.23.7.

Each particular area is analysed and, if necessary, tested with respect to load presumed to be
dangerous;asgiveninTable 34.23.8.

Particularareasaretestedatappropriatestagesoftheproject;asgiveninTable34.23.9.

Inrelevantcases,loadcombinationsareusedfortests;asgiveninTable 34.23.10.

Relevanttypesofloadcasesaretestedatrelevantstepsoftheproject;asgiveninTable34.23.11.

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Table34.232Effectsoflocalfailuremodesonglobalbehaviourofthestructure
Global
Matrix
Fibre
Cracks
Delamination Rigidity Loss Melting Debonding
Cracking
Rupture

Local

Matrix Cracking

Fibre Rupture
Cracks

Rupture

DX

PX

Delamination

Buckling

X
PX

Rigidity Loss

Melting
Debonding
Buckling

PX
X

X
X

Rupture
Key:

Propagation
D Dispersion
If local phenomena arise at given load, effects should be analysed and taken into account. The analysis should be based
on development tests and verified during qualification tests.

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Failure

Table34.233Detectionoftechniquestovariousfailuresoccurringduringtest
Test Means
Stress
Def.
Visual
ThermoEndoscopy
X-ray
C-Scan
AE.
Meas.
Meas.
Inspec.
graphy

Noise

Residual
Stress

Matrix Cracking

Destr.

Destr.

Fibre Rupture

Destr.

Destr.

Cracks

Delamination

Rigidity Loss

Melting
Debonding

Buckling

Burst

Rupture

Key:

Only if nominal or damage is external


Detected

Matrix cracking, fibre rupture, buckling, rigidity

m Loss of Modulus Loss detected if station gauges are well located


The relevant instrumentation has to be used in order to detect such phenomena.

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Failure

Table34.234Interrelationbetweenfailuremodesandtheirpossiblelocations
Location
Running
Sandwich
Stiffener
Local Load
Frame
Hole
Section
Edge
Edge

Reinforced Connection
Door
Parts

Matrix Cracking

Fibre Rupture

Cracks

Delamination
Rigidity Loss

Melting
Debonding
Buckling

Burst
Rupture
: Possible locations of failure should be specifically instrumented to allow the study of the phenomena.

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Failure
Matrix Cracking

Table34.235Interrelationbetweentypeofloadingandpossiblefailuremodes
Load
Residual
Acoustic
Static
Thermal
Dynamic
Fatigue
Stresses

Fibre Rupture

Cracks

Delamination

Rigidity Loss

Melting
Debonding

Impacts

Load History

Buckling

Burst

Rupture

Effects of these loads should be assessed and verified during tests.

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Table34.236Failuremodeswhichhavetobecoveredbythespecifictests
Test
Failure
DVPT
Qualif. Rupture Procurement Fabrication Proof*
Tests
Tests
Tests
Tests
Tests
Tests
Matrix Cracking

Fibre Rupture

Cracks

Delamination

Rigidity Loss

Useless

Melting

Debonding

Buckling

Burst

Rupture
Proof tests should not develop matrix cracking and if it is the case, the
Key:
effect should be taken into account in the dimensioning of the structure
and in the damage tolerance analysis.
Should be studied during development.
* Proof test necessity should be discussed.

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Instrumentation

Table34.237Appropriateinstrumentationofparticularareasofthestructure
Location
Reinforced
Pressurised
Stiffener
Frames
Holes
Local Load
Section
Edge
Doors

Stress Measurement

Definition Measurement

Connect
Parts

Visual Impact

Endoscopy

X-ray

C-Scan

Thermography

Acoustic Emission

Moir Method

Residual Stresses

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Table34.238Interrelationbetweenparticularareasofthestructuresandpossibledangerousloads
Load
Location
Residual
AE
Static
Thermal
Dynamic
Fatigue
Impact
Stresses
Running Section
Local Load

Sandwich Edge
Stiffener Edge

Frames
Holes

Reinforced Doors
Connection Parts

Load
History

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Location

Table34.239Testingofparticularareasofthestructure
Test
Procurement
DVPT Tests
Qualif. Tests
Rupture Tests
Tests

Running Section

Fabrication
Tests

Local Load

If possible

Sandwich Edge

Stiffener Edge

Frames
Holes

Reinforced Doors
Connection Parts

Proof Tests

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Load

Table34.2310Loadcombinationsfortherelevantcases
Load
Residual
Acoustic
Static
Thermal
Dynamic
Stresses

Residual Stresses

Acoustic

Static

Thermal

Fatigue

Impact

Dynamic
Fatigue
Impact

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Load

DVPT Tests

Table34.2311Testingdifferentloadcases
Test
Procurement
Qualif. Tests
Rupture Tests
Tests

Residual Stresses

Acoustic

If MS low

Static

Thermal

If MS low

Impact

Load History

Key:

Proof Tests

Dynamic
Fatigue

Fabrication
Tests

If any

If any
If any

In some sense

MS: Margin of safety

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34.24

Structural test reports

Theguidelinesindicatewhatcanreasonablybeexpectedtoappearinastructuralreport.
Theitemsincludedare:

Titlesheet:

distributionlist,

issue,

date.

Alterationsheet:

toincludeasummaryofchanges

Contentslist:

sectionnumber,

title,

issuenumber.

Summarypage

References:

applicablepapers.

Introduction:

structure,

purpose,

scope,

project.

Structuredescription

Designrequirements:

general,

specific,

uniquetoproject.

Materialslist:

propertyvalues,

sources,

qualities.

Analysismethods,forthoseusedinthereport.

FEMmodeldescription:Thisshouldbeclearandunambiguous.Ifnecessary,breakthemodel
into major subassemblies. Use FEM grids and structure or component drawings together as
superimposedorexplodedviews.

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Assumptions: Those made affecting the idealisations of the structure, e.g. load application,
modelling,staticanddynamicanalysis.

Results:Wherecomputerresults(e.g.FEM)areincluded,presentonlythosethathaveactually
beenused,orappearinsubsequentcalculations.

Analyses:

static,

dynamic.

Reservefactors(R.F.)ormarginofsafety(M.S.):Asummaryincludes:

drawing,partnumberortitle,

material,type,specificationnumberorgrade,

loadingcase,

load,momentandstresswithtype,appliedandallowableplusunits,

actualR.ForM.Svalue,

anyappropriateremarks,

locationwithinreportofassociatedcalculation,i.e.sectionorpagenumber.

Strengthanddynamicresponse:compliancestatementandconclusion.

Loadingcases:

list,

descriptions.

numberingsequence

Units:Statethoseusedinreport;preferablythesamethroughout.

Coordinatesystems,e.g.:

orientation,

locationoforigins,

Appendicesorannexes.

34.25

Analysis and test documents

34.25.1.1 Damage tolerance


34.25.1.2 General
All potential fracture critical items, PFCI, are analysed, and the analysis documentation, as a
minimum,containstheitemsdetailed.
Whentestingisusedinadditiontoanalysis,thetestmethodandresultsarealsoincluded.

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34.25.1.3 Safe life items


A description of the item with identification of the material used with full details of the method of
fabricationincludinglayup,e.g.numberofplies,theirsequenceandorientation;andaclearsketchof
allassumeddefectsanddamages.

Adescriptionoftheanalysisandtestperformed.Areferencetothestressreport.

Theloadingspectrumandhowithasbeenderived.

Materialdataandhowtheyhavebeenderived.

Environmentalconditionsandtheireffects.

Inthedemonstrationofnogrowthbehaviour,anylowstraincriterionusedarefullydescribed
andjustifiedwithappropriatesupportingtestevidence.

Demonstrationthattheintervalbetweenthetimeanydamagebecomesdetectabletothetimeat
which the extent of damage reaches the stated limits for the required residual strength
capabilityisatleastfourtimesthescheduledinspectionintervalintheapprovedmaintenance
plan.

Summaryofthesignificantresults.

34.25.1.4 Fail safe items


Thisincludesallitemsunderthatdefinitionandalsoincludesitemsinwhichspecialdesignfeatures
havebeenincurporatedanddemonstratedtobesatisfactory,inthattheyensurecrackarrestandare
capableofsustaininglimitloadsinthedamagedconditionbetweenregularlyscheduledinspections.
Forallfailsafeitems:

Adescriptionoftheitem;aspersafelifeitems,

Failuremodesassumed,

Stressanalysiswithnewloadingdistribution,

Fatigueanalysisofthemostcriticalitem,

Summaryofthesignificantresults.

34.25.1.5 Contained items


Adescriptionofthecontainmentanalysisincluding:

Velocityorenergyoftheitemasitstrikesthecontainingitem(shell),withworstcasesharpness
assumption,

Elasticorplasticshelldeformation,

Stressesintheshell,attachments,brackets,orothersimilaritemsduringimpact.

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34.26

References

34.26.1 General
[341]

C.N.E.S.
HSG110CNES,10.06.1988

[342]

J.D.Achenbach
Introduction:ThescienceandtechnologyofNDE
Chapter1,Flightvehiclematerials,structures,anddynamics
assessmentandfuturedirections
Vol.4TribologicalMaterialsandNDE
ASMEPublication,1992,ISBN0791806626

[343]

I.M.Daniel
NDEofcompositematerials
Chapter11,Flightvehiclematerials,structures,anddynamics
assessmentandfuturedirections
Vol.4TribologicalMaterialsandNDE
ASMEPublication,1992,ISBN0791806626

[344]

A.L.Siedl
InspectionofcompositestructuresParts1&2
Part1,SAMPEJnl,Vol.30,No.4,July/August1994,p3844
Part2,SAMPEJnl,Vol.31,No.1,January/February1995,p4248

[345]

0.Forli
Inorbitinserviceinspection
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AdvancedStructuralMaterials.March1990
ESASP303,p157162

[346]

S.K.Burkeetal
Nondestructivecharacterisationofadvancedcompositematerials
MaterialsForum(1994)18,p85109

[347]

R.Smith&C.Hobbs
TheneedforNDTofadvancedmaterials
14thInternationalEuropeanSAMPEConference,October1993
ISBN3952047708,p2534

[348]

X.E.Gros
ReviewofNDTtechniquesfordetectionoflowenergyimpactsincarbon
reinforcements
SAMPEJournal,Vol.31,No.2,March/April1995,p2934

[349]

H.Tretoutetal
ReviewofadvancedNDTmethodsforcompositesaerospacestructures
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p629634

126

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[3410]

J.Summerscales,Editor
NondestructivetestingoffibrereinforcedplasticscompositesVolume
2
ElsevierAppliedScience,ISBN1851664688,1990

[3411]

B.S.Wongetal
Ultrasonictestingofsolidfiberreinforcedcompositeplates
SAMPEJournal,Vol.30,No.6,November/December1994
p3640

[3412]

P.Cawley
Therapidnondestructiveinspectionoflargecompositestructures
Composites,Vol.25,No.5,1994,p351357

[3413]

G.R.Tillacketal
Inspectionperformanceinultrasonictesting
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p639644

[3414]

G.Bennettetal
Developmentofrealtimelowcosthighperformancescanningsystems
foradvancedultrasonicimaging
39thInternationalSAMPESymposium,April1114,1994
p13441355

[3415]

N.Wood
Largeareacompositeinspectionsystem(LACIS)automationof
traditionalinspectiontechniques
39thInternationalSAMPESymposium,April1114,1994
p13751390

[3416]

MightyMAUS
AerospaceAmerica,November1991,p4647

[3417]

Y.BarCohenetal
Compositematerialpropertynondestructivecharacterisationusing
obliquelyinsonifiedultrasonicwaves
39thInternationalSAMPESymposium,April1114,1994
p13161329

[3418]

N.Guo&P.Cawley
LambwavesfortheNDEofcompositelaminates
ReviewofProgressinQuantitativeNondestructiveEvaluation
Volume11B,1992,PlenumPress,ISBN030644206X
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M.Bashyam&J.L.Rose
Surfaceacousticwavetechniquesforceramicmatrixcompositematerials
characterization
ReviewofProgressinQuantitativeNondestructiveEvaluation
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20March2011
p14831490
[3420]

B.R.Tittmann
ExperimentaltechniquesinultrasonicsforNDEandmaterial
characterization
Chapter3,FlightVehicleMaterials,Structures,andDynamics
AssessmentandFutureDirections
Vol.4TribologicalMaterialsandNDE
ASMEPublication,1992,ISBN0791806626

[3421]

W.A.Grandia
Advancesinnondestructivetestingnoncontactultrasonicinspectionof
composites
39thInternationalSAMPESymposium,April1114,1994
p13081315

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W.Sachse&M.R.Gorman
Acousticemissionmeasurementsofaerospacematerialsandstructures
Chapter8,FlightVehicleMaterials,Structures,andDynamics
AssessmentandFutureDirections
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ASMEPublication,1992,ISBN0791806626

[3423]

G.M.Butyrin&A.V.Demin
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ESAWPP070,p673676

[3424]

JP.Monchalin
Laserultrasonics
Chapter4,FlightVehicleMaterials,Structures,andDynamics
AssessmentandFutureDirections
Vol.4TribologicalMaterialsandNDE
ASMEPublication,1992,ISBN0791806626

[3425]

JP.Monchalin
Progresstowardstheapplicationoflaserultrasonicsinindustry
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.12A,p495506,1993,PlenumPress,ISBN0306444836

[3426]

A.D.W.McKie&R.C.Addison
Rapidinspectionofcompositesusinglaserbasedultrasound
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.12A,p507516,1993,PlenumPress,ISBN0306444836

128

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[3427]

F.H.Changetal
Laserultrasonicinspectionofhoneycombaircraftstructures
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.12A,p611616,1993,PlenumPress,ISBN0306444836

[3428]

T.E.Drake
Laserultrasonictestingofaerospacematerials
39thInternationalSAMPESymposium,April1114,1994
p725739

[3429]

C.M.Scalaetal
Laserultrasonics:emergingtechnologyforaircraftNDE
NonDestructiveTestingAustralia
Vol.31,No.4,July/August1994,p9092

[3430]

J.F.Clarady&M.Summers
ElectronicholographyandshearographyNDEforinspectionofmodern
materialsandstructures
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.12A,p381386,1993,PlenumPress,ISBN0306444836

[3431]

G.DiChirico
Opticalmethodsfornondestructiveinspectionofstructural
components
TestingofMetalsforStructures,Naples,Italy,2931May,1990
p337343

[3432]

I.Cabezaetal
Thermaldistortionmeasurementonantennareflectorsbyrealtime
holographicinterferometryinambientpressure
ProceedingsoftheInternationalSymposiumonEnvironmentalTesting
forSpaceProgrammesTestFacilities&Methods
ESTEC,2629June1990,ESASP304,p403407

[3433]

H.U.Frey
HolographyAsuccessfultoolfordistortionmeasurementsonantennas
underspacesimulationconditions
ProceedingsoftheInternationalSymposiumonEnvironmentalTesting
forSpaceProgrammesTestFacilities&Methods
ESTEC,2629June1990,ESASP304,p395402

[3434]

J.F.Clarady
ElectronicholographicNDE
ReviewofProgressinQuantitativeNondestructiveEvaluation
Volume9,1990,PlenumPress,p10311038

[3435]

M.V.Raoetal
Dualvacuumstressingtechniqueforholographicnondestructive
testingofhoneycombsandwichpanels
NDTInternational,Vol.23,No.5,October1990,p267270

129

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[3436]

T.E.Tayetal
Applicationofholographicinterferometryinthedetectionofflawsin
compositeplates
AdvancedComposites93,InternationalConferenceonAdvanced
CompositeMaterials
Wollongong,Australia,1519Feb,1993,p683686

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P.Ferraroetal
Holographicinterferometryasinspectiontechniqueonaerospace
compositestructure
ProceedingsoftheInternationalSymposiumonSpaceApplicationsof
AdvancedStructuralMaterials.March1990
ESASP303,p151156

[3438]

G.Cavaccinietal
Detectionofimpactdamageincompositesbyholographic
interferometry
ProceedingsoftheInternationalSymposiumonSpaceApplicationsof
AdvancedStructuralMaterials.March1990
ESASP303,p145150

[3439]

G.B.Chaietal
Vibrationanalysisoflaminatedcompositeplates:TVholographyand
finiteelementmethod
CompositeStructures23(1993),p273283

[3440]

J.B.Deaton&R.S.Rogowski
Electronicshearography:currentcapabilities,potentiallimitations,and
futurepossibilitiesforindustrialnondestructiveinspection
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.12A,p395402,1993,PlenumPress,ISBN0306444836

[3441]

J.W.Newman
Productionandfieldinspectionofcompositeaerospacestructureswith
advancedshearography
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.10B,p212921331991,PlenumPress
ISBN0306439034

[3442]

J.W.Newman
Testcompositeswithlasers
MaterialsEngineering,July1992,p1011

[3443]

C.Hobbs
Theinspectionofaeronauticalstructuresusingtransientthermography
ProceedingsoftheNDTforCorrosioninAerospaceStructures
Conference,12Feb1992,6,1to6.10,ISBN0903409992

[3444]

T.Ahmedatal
Infraredthermalwavestudiesofcomposites
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.10B,p217321791991,PlenumPress

130

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ISBN0306439034
[3445]

W.P.Winfree
ThermalQNDEdetectionofairframedisbonds
NASACP3160,1991,p249260

[3446]

T.Jones&H.Berger
Thermographicdetectionofimpactdamageingraphiteepoxy
composites
MaterialsEvaluation,December1992,p14461453

[3447]

R.Danjouxetal
MECIR:AnewApparatusforthecontrolofmaterialsbyinfrared
thermography
SPIEVol1320InfraredTechnologyandApplications,1990
p282291

[3448]

C.P.Hobbsetal
Theapplicationoftransientthermographyforthenondestructive
testingandevaluationofaerospacematerials
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p645654

[3449]

E.G.Henneke&B.S.Tang
ThermalmethodsofNDEandqualitycontrol
Chapter6,FlightVehicleMaterials,Structures,andDynamics
AssessmentandFutureDirections
Vol.4TribologicalMaterialsandNDE
ASMEPublication,1992,ISBN0791806626

[3450]

J.Webber
NDTofCFRPstructures:evaluationofanewmethod
ProceedingsoftheInternationalSymposiumonSpaceApplicationsof
AdvancedStructuralMaterials.March1990
ESASP303,p163170

[3451]

S.Abbeetal
Suivideleffetdeviellissementenmilieuoxydantdematriaux
compositesC/SiCpardestechniquesnondestructives
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p687692

131

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[3452]

J.Bouteyreetal
Thicknessanddensitymeasurementofcarboncarbonmaterialsbyusing
backscatteringofXrays
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p655660

[3453]

M.P.Hentscheletal
NewXrayscanningtopographicapproachestonondestructive
evaluation
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures,March1992
ESASP336,p229232

[3454]

M.P.Hentscheletal
NewXrayrefractographyfornondestructiveinvestigations
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p661664

[3455]

R.A.Buchananetal
Digitalradiographyintheaerospaceindustry
Chapter7,FlightVehicleMaterials,Structures,andDynamics
AssessmentandFutureDirections
Vol.4TribologicalMaterialsandNDE
ASMEPublication,1992,ISBN0791806626

[3456]

C.Buenoetal
Highresolutiondigitalradiographyand3Dcomputedtomographyof
compositematerials
39thInternationalSAMPESymposium,April1114,1994
p766778

[3457]

L.Castaldelloetal
Advancedmaterialsnondestructivetestingusinghighresolutiondual
energytomography
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p635638

[3458]

D.Ekenhorstetal
Nondestructiveinspectionofceramicmatrixcompositescomponentsby
computerisedtomography
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p665672

[3459]

R.H.Bossietal
Xraycomputedtomographyfortheaircraft/aerospaceindustry
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.10B,1991,PlenumPress,ISBN0306439034,p21212127

132

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20March2011
[3460]

R.H.Bossietal
Xraycomputedtomographyofcomposites
26thInternationalSAMPESymposium,April1518,1991
p224238

[3461]

E.A.Birtetal
Imagingofimpactdamageingraphiteepoxycomposites
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.12A,p897904,1993,PlenumPress,ISBN0306444836

[3462]

R.H.Bossi&G.E.Georgeson
Appliedcomputedtomographyformaterials&processesdevelopment
39thInternationalSAMPESymposium,April1114,1994
p740753

[3463]

G.GeorgesonandR.Bossi
Xraycomputedtomographyforadvancedmaterialsandprocesses
InDevelopmentsinCeramicandMetalMatrixComposites
TheMinerals,Metals,&MaterialsSociety,1991,p143155

[3464]

R.Oster
Computedtomography(CT)asanondestructivetestmethodusedfor
compositehelicoptercomponents
Proceedingsofthe17thEuropeanRotorcraftForum
2427Sept1991,PaperERF9187

[3465]

P.D.Tonner&J.H.Stanley
Supervoltagecomputedtomographyforlargeaerospacestructures
MaterialsEvaluation,December1992,p14341445

[3466]

C.Bathiasetal
ApplicationofXraytomographytothenondestructivetestingofhigh
performancepolymercomposite.
ECCM6,Sept1993
WoodheadPublishing,ISBN1855731428,p617622

[3467]

B.A.Auld
ElectromagneticmethodsinNDE
Chapter5,FlightVehicleMaterials,Structures,andDynamics
AssessmentandFutureDirections
Vol.4TribologicalMaterialsandNDE
ASMEPublication,1992,ISBN0791806626

[3468]

G.E.McNeelege&C.Sarantos
RoboticNDEInspectionofadvancedsolidrocketmotorcasings
AIAA941222CP,p354366

[3469]

M.W.Siegel
Automationfornondestructiveinspectionofaircraft
AIAA941223CP,p367377

133

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20March2011
[3470]

R.Frankle&R.Menich
Eddycurrentinspectionofcompositematerials
39thInternationalSAMPESymposium,April1114,1994
p24512462

[3471]

X.E.Gros
Eddycurrenttesting:inspectingcompositematerials
MaterialsWorld,April1995,p180181

[3472]

M.P.DeGoeje&K.E.D.Wapenaar
Nondestructiveispectionofcarbonfibrereinforcedplasticsusing
eddycurrentmethods
Composites,Volume23,No.3,May1992,p147157

[3473]

D.W.Lowdenetal
Visualisingdefectgeometryincompositematerials
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p683686

[3474]

S.I.Ganchevetal
Microwavenondestructiveevaluationofthicksandwichcomposites
MaterialsEvaluation,April1995,p463467

[3475]

C.Wlfingeretal
Damagedetectionincompositematerialsbymonitoringelectrical
impedance
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures94,March1994
ESAWPP070,p677682

[3476]

A.C.Wey&L.W.Kessler
Quantitativemeasurementofdelaminationareainlowvelocity
impactedcompositesusingacousticmicroscopy
ReviewofProgressinQuantitativeNondestructiveEvaluation
Volume11B,1992,
PlenumPress,ISBN030644206X,p15631568

[3477]

L.J.Burnettetal
SolidrocketmotorNDEusingnuclearmagneticresonance
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.12A,1993,PlenumPress,ISBN0306444836,p663670

[3478]

G.Pfisteretal
Nondestructivetestingofmaterialsandcomponentsbycomputerized
tomographywithfastandthermalreactorneutrons
NuclearScienceandEngineering:110,p303315(1992)

[3479]

J.P.Komorowskietal
InspectionofaircraftstructuresusingDsight
39thInternationalSAMPESymposium
April1114,1994,p754765

134

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[3480]

J.P.Komorowskietal
ApplicationofDiffractosighttothenondestructiveinspectionof
aircraftstructures
ReviewofProgressinQuantitativeNondestructiveEvaluation
Vol.12A,1993,PlenumPress,ISBN0306444836,p449455

[3481]

P.Cawley
NDTofadhesivebonds
Chapter13,FlightVehicleMaterials,Structures,andDynamics
AssessmentandFutureDirections
Vol.4TribologicalMaterialsandNDE
ASMEPublication,1992,ISBN0791806626

[3482]

T.Pialucha&P.Cawley
Thedetectionofaweakadhesive/adherendinterfaceinbondedjointsby
ultrasonicreflectionmeasurements
ReviewofProgressinQuantitativeNondestructiveEvaluation
Volume11B,1992
PlenumPress,ISBN030644206X,p12611266

[3483]

P.N.Dewen&P.Cawley
Anultrasonicscanningtechniqueforthequantitativedeterminationof
thecohesivepropertiesofadhesivejoints
ReviewofProgressinQuantitativeNondestructiveEvaluation
Volume11B,1992
PlenumPress,ISBN030644206X,p12531260

[3484]

D.R.Prabhu&W.P.Winfree
Automationofdisbonddetectioninaircraftfuselagethroughthermal
imageprocessing
ReviewofProgressinQuantitativeNondestructiveEvaluation
Volume11B,1992
PlenumPress,ISBN030644206X,p13231330

[3485]

D.W.Lowden
Quantifyingdisbondarea
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures,March1992
ESASP336,p223228

[3486]

P.Plotard&C.LeFloch
Nondestructiveinspectionofcarboncarbonwithadaptedcoatingfor
oxidation
ProceedingsoftheInternationalSymposiumonSpaceApplicationsof
AdvancedStructuralMaterials.March1990
ESASP303,p171180

135

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20March2011
[3487]

G.Y.Baaklinietal
NDEoftitaniumalloyMMCringsforgasturbineengines
DEVol.55,Reliability,StressAnalysis,andFailurePrevention
ASME1993,ISBN079181172250,p239250

[3488]

H.Trtoutetal
Infraredthermographydevelopmentformaterialevaluationofhermes
spaceplanecomponents
ProceedingsoftheInternationalSymposiumonSpaceApplicationsof
AdvancedStructuralMaterials.March1990
ESASP303,p181186

[3489]

G.Salaetal
Specialproblemsof3DultrasonicQNDItechniquesandapplicationsto
compositeaerospacestructures
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures,March1992
ESASP336,p209216

[3490]

Integritycontrolforhightemperaturestructuralapplications
DaimlerBenzAerospaceDornierReports
PhaseIFinalReport,November1993
PhaseIIFinalReport,February1995
ESTECContract9907/90/NL/PP(SC)

[3491]

R.W.AvanderVen&H.Bolks:Fokker,NL.
AircoupledultrasonicCscan(AIRSCAN)fornondestructive
inspection
ESAConferenceonSpacecraftStructures,Materials&Mechanical
Testing,March1996.Abstracts,p94

[3492]

W.A.Grandia&C.M.Fortunko:QMI/NIST,USA
NDEapplicationsofaircoupledultrasonictransducers
IEEEInternationalUltrasonicsSymposium,Seattle,710November,1995

[3493]

ESAPSS03207Guidelinesforcarbonandotheradvancedmaterial
prepregprocurementspecifications.

[3494]

J.O.Strycek&H.Loertscher:QMIInc.,USA.
Ultrasonicaircoupledinspectionofadvancedmaterial
NDTNet.Vol.4No.12,December1999.

[3495]

UltrasonicSciencesLtd.,UK
Multiaxisautomaticultrasonicinspectionsystemsforadvanced
compositeaircraftstructures.
Privatecommunication2003.

[3496]

M.C.Bhardwaj&GFStead
Phenomenaladvancementsinnoncontactultrasoundforcomposites
characterisation
46thInternationalSAMPESymposiumMay610,2001

136

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20March2011
[3497]

J.S.McIntoshetal.,
Thecharacterisationofcapacitivemicromachinedultrasonictransducers
inair
Ultrasonics40(2002)p477483.

[3498]

M.Castaings&B.Hosten
TheuseofElectrostatic,Ultrasonic,AircoupledTransducerstoGenerate
andReceiveLambWavesinAnisotropic,ViscoelasticPlates
Ultrasonics,v.36,p361365(1998).

[3499]

E.Bloomeetal.
RecentobservationswithaircoupledNDEinthefrequencyrangeof650
kHzto1.2MHz
Ultrasonics40(2002)p153157.

[34100] R.Stoesseletal.
Aircoupledultrasoundinspectionofvariousmaterials
Ultrasonics40(2002)p159163
[34101] J.Poguetetal.
Phasedarraytechnology:Concepts,probesandapplications,8th
EuropeanCongressonNondestructivetesting,June1721,Barcelona,
Spain.2002
[34102] Mahautetal.
Developmentofphasedarraytechniquestoimprovecharacterisationof
defectlocatedinacomponentofcomplexgeometry
Ultrasonics40(2002)p165169
[34103] J.Penaetal.
Lowcost,lowfrequencyphasedarraysystemfordamagedetectionin
panels
Proceedingsofthe2ndEuropeanworkshoponstructuralhealth
monitoring,2004
[34104] M.J.S.LoweandP.Cawley
TheApplicabilityofPlateWaveTechniquesfortheInspectionof
AdhesiveandDiffusionBondedJoints
JournalofDestructiveEvaluation,Vol13,No4,1994
[34105] R.Seifried,L.J.Jacobs&J.Qu
CharacterizationofadhesivebondpropertieswithLambWaves
ReviewofProgressinQuantitativeNondestructiveEvaluationVol.20,
EditedbyD.O.ThompsonandDEChimenti
[34106] P.B.Nagy&L.Adler
Nondestructiveevaluationofadhesivejointsbyguidedwaves
JApplPhys.66(10),15november1989
[34107] M.Lemistre&D.Balageas
StructuralhealthmonitoringsystembasedondiffractedLambwave
analysisbymultiresolutionprocessing

137

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20March2011
SmartMaterialsandStructures10(2001)p504511
[34108] P.Frommeetal.
Aguidedwavearrayforstructuralhealthmonitoring
Proceedingsofthe2ndEuropeanworkshoponstructuralhealth
monitoring2004

34.26.2 ECSS documents


[See:ECSSwebsite]

ECSSQST20
ECSSEST30series
ECSSEST3201

SpaceproductassuranceQualityassurance;
previouslyESAPSS0120
SpaceengineeringMechanical
Fracturecontrol;previouslyESAPSS01401

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35
Objective of verification
35.1

Introduction

35.1.1

General

Theobjectiveofverificationisstatedalongwiththoseadditionalfactorswhicharetobeconsidered
for structures manufactured from fibrereinforced composite materials compared with metal
structures.

35.1.2

Composite structures

35.1.2.1

Key factors

Toverifyacompositestructure,itemswhichareconsideredare:

Adequacyofdesign,

Manufacturing,and

Testing.

35.1.3

Composite materials

35.1.3.1

Additional factors

Inadditiontotherequirementsofametallicdesign,thefactorsspecifictocompositesare:

Procurementspecification:Adetailedspecificationforalltherawmaterial(s),e.g.

prepregs,

resins.

Incomingcontrol:Procedureforallrawmaterials

Design allowables:Philosophyofassessment.

Tests:Tosupportthecompositedesign.

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Manufacturing:

Procedureforallparts.

Curingprocessprocedure.

Assembly:Procedurefortheassemblyofthestructure.

35.1.3.2

Verification procedure

Theverificationprocedurecomprisesof:

Hardware,and

Software,e.g.assessmentofdesignallowables.

35.1.3.3

Verification guidelines

A general verification procedure for composite structures can be derived from the guidelines given
for:

Rawmaterials,[See:Chapter36].

Design allowables,[See:Chapter37].

Theguidelinesprovidethefundamentalsforagivenprocedure.

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36
Procurement specifications for raw
materials
36.1

Introduction

36.1.1

Guidelines

The guidelines presented contain information to assist in the preparation of specifications for the
procurement of advanced composite constituents and prepregs. Also described are the parameters
thatitisnecessarytocontrolormonitorforqualificationandbatchcontrol.
The guidelines are not intended to be definitive specifications. In many cases, it is not necessary to
specify all the parameters outlined. It remains the judgement of those preparing a specification to
includeonlywhatisreallynecessary,therebyavoidinganexcessivelycomplexspecificationandthe
undulyhighcostofcomplyingwiththem.

36.2

Specification methods

36.2.1

Fiche sheet principle

36.2.1.1

General

There is a tendency for specificationsto be written on what is tautologicallydescribed asthe fiche


sheetprinciple.
Thestructurehasobviousbenefitsforahardwaremanufacturerusinganumberofprepregmaterials.
Unfortunately, the system is fraught with practical difficulties, which become apparent when a
particular material needs a special test or when various manufacturers are persuaded to supply a
materialtothesamespecificationprocedure.
However, the trend towards the fichesheet specification structure is growing, owing to the
reductioninpaperworkandadministrativeeffortthatitaffords.

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36.2.1.2

Master document

The fichesheet structure needs the creation of a master document in which items are defined,
including:

Ordering,

Delivery,

Qualification,

Acceptance,

Batchrelease,and

Testmethodprocedures.

Itdoesnotincludespecificnumericalpropertydatarequirements.

36.2.1.3

Fiche sheet

Aseparatedocumentthefichesheetisissuedasasupplementtothemasterdocumentandlists
therequiredpropertydataforaspecificmaterial.

36.2.2

Specific material specification

Owing to problems identified with the fichesheet principle, most materials are still ordered to a
specific material specification, which is established by the manufacturer and customer in
collaboration.

36.3

Guidelines on resin procurement

36.3.1

Scope

The guideline gives information on the preparation of a specification for the procurement of a
particularresinsystem.
The main items which are needed for the identification of requirements for batch control and the
qualificationofaresinsystemarelisted.

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36.3.2

Basic information to be provided by the supplier

36.3.2.1

Introduction

Whereconstituentitemsareorderedseparately,theassociatedinformationissuppliedforeachitem,
i.e.:

General;asshowninTable 36.3.1.

Base resin;asshowninTable 36.3.2.

Hardener;asshowninTable 36.3.3.

Catalyst;asshowninTable 36.3.4.

Modifier;asshowninTable 36.3.5.

Solvent;asshowninTable 36.3.6.

Blend;asshowninTable36.3.7.

Thesupplieralsoconfirmsthatthematerialisfreefromcontamination.
Alltheinformationrequirementsdescribedarefortheapprovalofthematerial.Allthosemarkedwith
an asterisk are needed for batch control. If one or more of the mentioned parameters is out of
specification,certainretestingcanberequired.

36.3.2.2

General

All the information described in Table 36.3.1 are for the approval of the material. All those marked
withanasteriskareneededforbatchcontrol.

Table36.31Resinprocurement:GeneralInformation

Information

Batch

1.
2.
3.
4.
5.
6.
7.

Manufacturer's name and product name


Procurement specification number
Batch number and the identification numbers as required
Release date
Packaging requirements
Storage and transportation constraints
Allowable shelf life

*
*
*
*
*
*
*

*Necessaryaspartofabatchtest

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36.3.2.3

Base resin

All the information described in Table 36.3.2 are for the approval of the material. All those marked
withanasteriskareneededforbatchcontrol.

Table36.32Resinprocurement:Baseresin

Information

1.

Chemical compliance: supply of infrared (I.R.) spectrum


analysis
Density
Solids content or volatile content
Viscosity or melting point
Epoxy content or equivalent
Refractive index (only for liquids)

2.
3.
4.
5.
6.
Key:

ifapplicable

*Necessaryaspartofabatchtest

Batch

*
*
*
*
*

36.3.2.4

Hardener

All the information described in Table 36.3.3 are for the approval of the material. All those marked
withanasteriskareneededforbatchcontrol.

Table36.33Resinprocurement:Hardener

1.
2.
3.
4.
5.
6.

Information

Chemical compliance: supply of I.R. spectrum analysis


Density
Volatile or solids content
Amine number or anhydride value or nitrogen content
Viscosity or melting point
Refractive index (only for liquids)

Batch

*
*
*
*
*

*Necessaryaspartofabatchtest

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36.3.2.5

Catalyst

All the information described in Table 36.3.4 are for the approval of the material. All those marked
withanasteriskareneededforbatchcontrol.

Table36.34Resinprocurement:Catalyst

Information

1.
2.
3.
4.
5.
6.

Chemical compliance: supply of I.R. spectrum analysis


Density
Solids content or volatile content
Viscosity or melting point
Epoxy content or equivalent
Refractive index (only for liquids)

Key:

ifapplicable

*Necessaryaspartofabatchtest

Batch

*
*
*
*

36.3.2.6

Modifier

All the information described in Table 36.3.5 are for the approval of the material. All those marked
withanasteriskareneededforbatchcontrol.

Table36.35Resinprocurement:Modifier

1.
2.
3.
4.

Information

I.R. Spectrum
Density
Viscosity or melting point
Refractive index (only for liquids)

Batch

*
*
*

*Necessaryaspartofabatchtest

36.3.2.7

Solvent

All the information described in Table 36.3.6 are for the approval of the material. All those marked
withanasteriskareneededforbatchcontrol.

Table36.36Resinprocurement:Solvent

1.
2.
3.

Information

Density
I.R. Spectrum
Refractive index

Batch

*
*

*Necessaryaspartofabatchtest

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36.3.2.8

Blend

All the information described in Table 36.3.7 are for the approval of the material. All those marked
withanasteriskareneededforbatchcontrol.

Table36.37Resinprocurement:Blend

Information

Batch

Uncured
(priortoreleaseforproductionuse)

1.
2.
3.
4.
5.

Gel time at defined temperature


Viscosity versus temperature, or
Viscosity versus time at defined temperature
Density
Heat of polymerisation

*
*
*

Cured

1.
2.
3.
4.
5.
6.

Glass transition temperature


Density
Shrinkage due to curing
Water absorption
Outgassing
Radiation effects

*Necessaryaspartofabatchtest

36.3.2.9

Thermo mechanical properties

Thedeterminedpropertiesare:

Compressionstrength.

Compressionmodulus.

Tensilestrength.

Tensilemodulus.

Elongation.

Impactstrength.

Poissonsratio.

Hardness.

Density.

Coefficientofthermalexpansion,CTE.

Shearmodulusversustemperature.

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Thesupplierindicates:

thetypesoftestingusedtoestablishtheproperties,and

theirtypicalvalues,and

thelikelypropertyvariationthatcanbeexpected.

36.4

Guidelines on carbon and other fibre prepreg


procurement

36.4.1

Scope

36.4.1.1

General

Theguidelinesdescribetheparameterswhicharenecessarytocontrolormonitorprepreginorderfor
validationandbatchcontrol..
Fordetailedinformation,refertoESAPSS03207.

36.4.1.2

Thermosetting resin matrix

The guidelines are intended as a general guide for organisations preparing specifications for the
procurementofparticularthermosettingresinimpregnatedreinforcingfibresystems(prepreg).

36.4.1.3

Thermoplastic matrix

Whilst the guidelines concentrate on the procurement of thermosetting resin prepreg they are, in
manyrespects,alsoapplicabletothermoplasticmatrixprepreg.

36.4.2

Description and classification of prepreg

36.4.2.1

Fibre type

Theguidelinesareaimedprimarilyatpurchasersofprepregcontainingcarbonfibres.However,many
oftheparametersdescribedareapplicabletoprepregsofothercontinuousreinforcingfibres,suchas
glass,boron,aramids,siliconcarbideandalumina.

Hybrid prepregs, containing a mixture of reinforcing fibres, such as glass and carbon, also need
similarspecificationcontrol.

36.4.2.2

Prepreg type

The most common type of prepreg is the unidirectional (UD) variety. A unidirectional prepreg
contains a parallel planararray offibres,usually several fibres thick, suitably preimpregnated with
eitherapartiallycuredoranuncuredspecifiedthermosettingresin.
Prepregs incorporating woven arrays of reinforcing fibres, i.e. fabrics, are an important group of
materials.Thepropertiesofthefibreandresinconstituentsoftheprepregcanbedefinedbyreference
toappropriatespecificationsfortheseconstituents.

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36.4.2.3

Resin type

[See:36.3forguidelinesonproducingaresinprocurementspecification]

36.4.2.4

Prepreg classification

Laminationofprepregpliesandcuringunderdefinedconditionsoftemperature,pressureandtimein
amouldingpressorautoclaveproducecomponentswithrequiredstrengthorstiffnesscharacteristics.
Theclassificationofaprepregcanbeintermsof:

Therequiredmechanicalpropertiesofacuredlaminate,frequentlyspecifiedtobethoseatthe
operatingtemperatureandhumidityofacomponent,or

Thetypeofresinorfibrecanbeusedasabasisforprepregclassifications.

In either case, the material supplier provides guidelines on the range of applicability of a particular
prepreganditsconstituents.

36.4.2.5

Thermoplastic matrix prepregs

Thesearesuppliedinunidirectionalandfabricformsbutdonotpossessthesameintrinsicphysical
characteristicsofthermosetprepregs.Thermoplasticprepregstendtohave:

Poordrape,and

Notack.

Aprocurementspecificationofthermoplasticmatrixprepregscontainsfewerrequirementsthanthose
forthermosetprepregs.Factorsrelatingtomaterialcontentanddistributionareimportantbutthose
relatingtomatrixchemistryarelesscritical.

36.4.3

Prepreg charachteristics for qualification and batch testing

36.4.3.1

Specification

Itisenvisagedthatallthecharacteristicsdescribedsatisfytheapprovalofaprepregtoaspecification.
Many of the requirements are necessary for batch release to a specification. It is usually the
responsibility of the user to define a schedule of acceptance tests to ensure that released material
complieswiththespecificationtowhichitisreleased.
Itisfurtherenvisagedthattheconstituentresinandfibresystemintheprepreghavebeenvalidated,
batchreleasedandacceptedaccordingtoappropriatespecifications.
Aprocurementspecificationdefinesalltheitems.

36.4.3.2

Identification and marking

A specification usually defines the way in which a consignment of prepreg is identified by the
manufacturer.Therequirementsforreeledprepregtapeandcutunidirectionalprepregsheetareoften
slightlydifferent.

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36.4.3.3

Release documentation

It is usual practice for information additional to that set out in Identification and Marking to be
suppliedasreleasedocumentationaccompanyingeachbatchorshipment(whicheveristhesmaller)
ofmaterialreleasedtoaspecification.

36.4.3.4

Packaging

Bothfacesofaprepregareprotectedbynonmigratory,noncontaminatingbackingmaterials.

36.4.3.5

Prepreg construction

Theconstructionparametersofaprepregthatarecommonlyspecifiedare:

Thickness

Cohesion

Gapsandslits

Splicing

Dimensions:

width,

length.

Resincontent

Fibrecontent

Prepregmass

Volatilecontent

Tack

Edges

Flammability,toxicityandsafety

Shelflifeandshoplife

Fabricparameters:

weavetype

arealweight

warpandweftcharacteristics

Characteristicsasprovidedby:

HPLC

DSC

DMA

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36.4.3.6

Prepreg quality and defects

Prepregmaterialassuppliedinevitablyexhibitssomedefects.
Thedefinitionofdefectivematerialisasignificantareaderivedbyagreementbetweenmanufacturer
andcustomer,andcaninclude:

Discontinuoustows(excludingallowabletowsplices),

Prepregsplices,

Curedorhardenedresinparticles,

Fibrestarvedareas,

Resinvariations:

excessresin,or

resinstarvedareas,

Gapsorslits(inexcessofthosedefined),

Whorls,

Fuzzballs,

Anyimperfectioninfibrealignmentduetotowslackness:

kinks,

waves,or

twistedfibres.

Foreignmaterial,

Contamination,and

Anyotherfeaturesthatadverselyaffectitsperformance.

36.4.3.7

Batch acceptance testing by the supplier

Itemstobedefinedare:

Testparameters,

Batchacceptanceandrejectioncriteria,and

Retestconditions.

36.4.3.8

Incoming inspection by the user

It is common practice for a user to check incoming material by retesting for some or all the batch
acceptancerequirements.
Retestingisattheusersdiscretionandisnotnormallyincorporatedintoaprocurementspecification.

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36.4.4

Laminate Characteristics

36.4.4.1

Minimum properties

Itisusualpracticetospecifyminimumphysicalandmechanicalpropertiesforalaminateproduced
fromtheprepregbymeansofadefinedcureschedule.

36.4.4.2

Cure schedule

The defined cure schedule is for specification purposes and need not correspond to the component
production cure; it is, however, within acceptable temperature limits. A number of curing cycle
repetitionshavingnoadverseinfluenceonthelaminatemechanicalpropertiescanbeincorporated,if
necessary.
Parametersandtheirinterrelationshipstobedefinedare:

Curetime(withallowablerange);

Curetemperature(withallowablerange);

Permissiblerangeofheatupandcooldownrates;

Curepressurerangeorcycling;

Preandpostcuredwellphasesandtheirpurpose.

36.4.4.3

Manufacturing factors

Ifsodesired,itemsforthepreparationoftestlaminatescanallbespecified,e.g.:

Tooling,

Prepregstackingsequence,

Releaseandbleedclothlayers,and

Stackassemblyforpreparingtestlaminates.

Thesamplecuttingpatternfromthelaminatecanalsobespecified.Itistheconventionalpracticeto
manufactureunidirectionallyreinforcedlaminatesforspecificationtestingpurposes.Specialtestscan
benecessaryinthecaseofwovenfibreprepreg.

36.4.4.4

Qualification testing

Various mechanical and physical properties are determined at ambient temperature and humidity
againstdefinedteststandardsagreedbetweenthesupplierandpurchaser.Theseinclude:

Longitudinaltensilestrength

Longitudinaltensilemodulus

Longitudinalcompressivestrength

Longitudinalcompressivemodulus

Transversetensilestrengthandmodulus

Transversecompressivestrength

Longitudinalflexuralstrengthandmodulus

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Transverseflexuralstrengthandmodulus

Shortbeamshearstrength(interlaminarshearstrength)

Fibrevolumefractionandvoidcontent

Laminatedensity

Laminateoutgassingandoffgassingperformance

Flammability

Toxicity

Ifnecessary,additionalelevatedtemperatureorhumidityconditionscanbeprescribed.

36.4.4.5

Batch and incoming inspection testing

Guidelinesaresuggestedasapracticalminimumforrealisticqualitycontroltestingofaprepreg,for
approval,batchandincomingacceptancepurposes.
Other laminate tests can be defined to reflect the service conditions, e.g. compression or elevated
temperaturetests.
Usually,aminimumoffiveindividualtestsforeachpropertyarecarriedout,theindividualresults
arerecordedaspartofthereleasedocumentation.

Fibrevolumefraction:Tobewithinaspecifiedtolerance,usuallyabout3%ofadefinedfigure
intherange60to65%.

Longitudinal flexural strength: To be greater than a defined minimum, with a specified


maximumcoefficientofvariationofresults,usuallyabout6%.

Longitudinal flexural modulus: To be within a defined range, with a specified maximum


coefficientofvariationofresultsofusuallyabout6%.

Interlaminar shear strength: To be within a defined range at ambient temperature and to be


greaterthanaspecifiedminimumatadefinedelevatedtemperature,withaspecifiedmaximum
coefficientofvariationofresults,usuallylessthan10%.

Thevaluesquotedaretypicalforcarbonfibreprepreg.

36.4.5

Test methods

Unfortunately, it is not feasible to give fully explicit guidance on applicable test methods for
incorporation into specifications. Practices vary considerably from country to country and from one
compositehardwareconstructortothenext.
Probably the most comprehensive range of applicable test methods is that published by ASTM and
ANSI,buteventhisisnotexhaustive.
For some properties, e.g. prepreg tack, no national standard test methods have been published: the
nonstandardonesthatdoexisthaveoftenbeenwrittenespeciallyforspecificationpurposes.

[Seealso:Chapter7fortestmethods;ESAPSS03207Appendix2]

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36.5

References

36.5.1

ECSS documents
[See:ECSSwebsite]

ECSSEST3208
ECSSQST70
ECSSQ7071

Materials
Materials,mechanicalpartsandprocesses
Datafortheselectionofspacematerialsand
processes

36.5.2

ESA publications

ThedocumentscitedhavenotyetbeentransferredtotheECSSdocumentationsystem.

ESAPSS03207

Guidelineforcarbonandotheradvancedfibre
prepregprocurementspecification

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37
Philosophy of assessment of design
allowables
37.1

Introduction

Design allowables are defined, [See: 37.3], and a procedure for the generation of allowable data for
developmentpurposesisprovided,[See:37.4].

Testdataforacarbonfibre/epoxycompositeisincluded,[See:37.5].

37.2

Carbon fibre reinforced plastics

37.2.1

Design values

37.2.1.1

General

Strengthisverifiedbyanalysisunderusageofmaterialdatawhichisachievedwithaprobabilityof
99%onaconfidencelevelof95%,i.e.Avalues.
MILHDBK5,Ref.[372],givesinformationonhowthosedesignvaluescanbegeneratedwithbatch
tobatchvariationanddeliveriesfromdifferentsuppliers.Thenecessaryinformationinthisrespectis
notavailableandconsequentlytheapproachofMILHDBKcannotbeformallyapplied.Furthermore,
the extension to different suppliersis considered asnot justified if a materialis used onlyfrom one
source.

37.2.1.2

Procedure

ToovercometheproblemshighlightedwithrespecttoMILHDBK5,aprocedureisoutlinedonhow
to generate design allowables for unidirectional CFRP elements, manufactured from 914C/HM, 0.1
mmthickprepregs.
TheprocedureintentionallycoversthevariabilityofCFRPmaterialanddefinesdesignvalueswhich
can be achieved also in future manufacture, provided that the defined quality assurance provisions
aretaken.

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37.3

Definition of design allowables

37.3.1

'A' basis allowable

At least 99% of the population of values is expected to equal or exceed the A basis mechanical
propertyallowable,withaconfidenceof95%.

37.3.2

'B' basis allowable

At least 90% of the population of values is expected to equal or exceed the B basis mechanical
propertyallowable,withaconfidenceof95%.

37.4

Development procedure

Mechanical properties, relevant for an actual application, are often not tested during incoming
inspection. If they are, the values obtained from a few samples do not enable the generation of A
basisdesignallowables,[Seealso:37.3].
Inordertoobtaindatawhichcanbeusedduringthedevelopment,thepolicytobeimplementedis:

Theminimumacceptancevalueofasmallsampleisconsideredasthelowestaveragevalueof
anybatchaccepted.

Based upon present knowledge, the minimum values (99% probability of exceedance) are
estimatedunderindividualconsiderationoftheirtypicalscatterwithonebatch.

ThedataofamediumsizesampleareconsideredasnormallyhavingaGaussiandistribution.A
slightreservefactorcoveringuncertaineffectsonscatterofapproximately5%hasbeenapplied
additionally,butwhichcanberemovedifenoughstatisticaldatabecomeavailableintime.

Thedesignallowablesarenotjustifiedbythesupplier.Thisresultsinhighcostandpossibly
delaysindelivery.Testing,wherenecessary,istheresponsibilityoftheuser.Therefore:

Receiving inspection is based on low sample numbers against acceptance values which
needtobeexceededbyallthespecimensinsmallsamplesize;6specimens.

Thecustomerperformsadditionalmaterialtestingtoestablishthestatisticaldistribution.
Thiscanenableacceptanceofabatchwhichdoesnotmeettheacceptancerequirement,
butcanshowlowerscatterwithinthebatch.

37.5

Test data

37.5.1

Material

Thetestdatapresentedareforthehighmodulus,HM,carbonfibre/epoxysystem:

Prepreg914CMS440:batch75/51487

FibrechargeE2M352.

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37.5.2

Data

37.5.2.1

General

Table37.5.1givesthepropertiesofthematerialobtainedfromtests.Thestatisticalbasedprobability
ofexceedancedataforthesamebatchofmaterialaregivenfor:

TensilestrengthUD0inFigure37.5.1.

TensilestrengthUD90inFigure37.5.2.

CompressionstrengthUD0inFigure37.5.3.

InterlaminarshearstrengthUD45inFigure37.5.4.

Table37.51TestdataforHMcarbon/epoxyspecimen

Tensile:
UD 0
Tensile:
UD 90
Compression:
UD 0
Interlaminar
shear strength:
0/45

SD

(mmxmm)

(N/mm2)

(N/mm2)

1x7

1121

122

738

45.6

5.8

27.3

898

45

756

64.5

7.8

40.0

SpecimenCross
section

R1tu

R1cu

Cross-section at
Failure
Facing
0.2 x 25

R13su (0/45

2.3 x 10

R2tu

Key:

Fourpointsandwichbending.

Values,excludingILS,relateto60%byvolumefibrecontent.

99%/95%
Values
(N/mm2)

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37.5.2.2

Tensile strength UD 0, batch 352

Figure37.51Probabilityofexceedance:Tensilestrength0

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37.5.2.3

Tensile strength UD 90, batch 352

Figure37.52Probabilityofexceedance:Tensilestrength90

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37.5.2.4

Compression strength UD 0, batch 352

Figure37.53Probabilityofexceedance:Compressivestrength90

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37.5.2.5

Interlaminar shear strength UD 45, batch 352

Figure37.54Probabilityofexceedance:Interlaminarshearstrength

37.6

References

37.6.1

General
[371]

MBB/ERNO
Unpublishedwork

[372]

MILHDBK5F:Metallicmaterialsandelementsforaerospacevehicle
structures
November,1990

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38
Manufacturing techniques
38.1

Introduction

38.1.1

Processing techniques

Fibrereinforcedplasticscanbeprocessedbyanumberofmethods,Ref.[381],[382].
The majority of composite space structures are assembled from prepreg configurations, which are
laidupbyhandandthenmouldedinanautoclave,[See:38.4].
Filament winding, [See: 38.5], is also used, mainly for cylindrical configurations, [See also: Chapter
29].Variantsofthesewidelyacceptedprocessmethodsaredescribed.
Supportingprocesstechnologiesarealsodescribed.Theseinclude:

Resintransfermoulding,[See:38.7].

Pultrusion,[See:38.8].

Pressureforming,[See:38.10].

Information is also provided on developing technologies which have a possible future use, such as
radiationcuring,[See:38.12].

38.1.2

Process selection

Theselectionofasuitableprocessisinfluencedbyavariousfactors,including:

Designofstructure,

Materialsselection,

Equipmentavailability,

Componentconfiguration,

Unitnumbers,and

Costtomasstradeoffs.

The selection of a manufacturing route is often the result of a tradeoff between a minimum mass
designandacceptablecost.
[Seealso:ECSSQST70;ECSSQ7071]

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38.2

Process selection criteria

Theselectionofaprocessis,intheory,determinedbyidentifyingthemostcosteffectivesolutionfor
thedesiredstructuralconfiguration.Thisisanidealisedassumptionwhichisbasedontheexpectation
thatthereisalsoanoptimumtechnicaldesignsolutionfortheapplication.
Inreality,anumberofdesignsareusuallyabletofulfiltheperformancespecification,Ref.[383].
Forexample,acceptabledesignconfigurationsforthrustcylindershavebeenproducedby:

Sandwichconstructionswithcompositefaceskinsandlightalloyhoneycombcores,

RibstiffenedmonolithicCFRPdesigns,and

FilamentwoundCFRParrangements,Ref.[384],[385].

Theselectionofaprocessisdrivenbyanumberofconsiderations,ofwhichthemainonesare:

Canpreviousdesignsandmanufacturingexperiencebeusedtofindasolution?

Foranewdesignconcept,isthereaccesstoappropriatemanufacturingfacilities?

Doestheprocessenableanoptimumfibreorientationandfibrevolumefractiontobeachieved?

Doestheprocessachievethedesiredcomponentshapeanddimensionaltolerances?

Whatisthepartcountfortheidentifiedprocessroute?

Whatarethesubsequentmachiningandfinishingoperationsaftercomponentprocessing?

Cantheprocessaccommodateloadintroductionpointsincomponents?

For design and quality control purposes, what material property data from the process route
needstobeobtained?

What are the cost implications with respect to manhours, tooling, consumable materials and
processtimes?[Seealso:Chapter40]

The selection of a manufacturing route is often based on tradeoffs between competing designs to
minimisemassandacceptablecosts.

38.3

Hand lay-up

38.3.1

General

Fibrereinforcedplasticsprocessinghastraditionallyinvolvedthemanuallayupofmaterials.Thisis
oftentheonlyroutepossiblewhenlownumbersofitemsaremadetoanyonedesign.Whenthescale
of manufacturing operations increases, the amount of manual involvement can be reduced by
automation. The aim is to reduce costs and improve product consistency. Automated and
programmableprepregcuttingsystemswereintroducedonthisbasis.
Manuallayupisusedin:

wet laminating,and

prepreg lay-up,priortoautoclaving.

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38.3.2

Wet lamination

38.3.2.1

General

Wetlayupbyhandisamethodofmouldingcomponentsatroomtemperatureusingthermosetting
polyester and epoxy resins, usually with mat or woven roving reinforcements. A chemical reaction,
initiatedintheresinbyacatalyticagent,produceshardeningoftheresininthefinishedpart.

38.3.2.2

Process

Themouldandthegelcoveringareproperlyprepared.Choppedstrandmat,clothorwovenrovings
are cut to shape from reels using a utility razor knife, large scissors or an electric clothcutting
machine.
Measuredamountsofresinandcatalystarethenthoroughlymixedtogether.Theresinmixturecanbe
appliedtothereinforcementeitheroutsidethemouldorinsideit.Toensurecompleteremovalofair
and wetout of the fibres, the resin is applied first and the reinforcement is placed on top. Brushes,
squeezersandrollersareusedtocompactthematerialagainstthemouldsurfaceandtoremoveany
entrappedair,asshowninFigure38.3.1.

Figure38.31Handlayupprocessformatorcloth
Additional layers of mat or woven roving can then be applied until the total thickness has been
achieved. Layers of mat and woven roving are usually alternated to ensure good interlaminar
bonding,toavoidairentrapmentandtoensurethehigheststrength.
Fibrevolumecontentsvarywiththereinforcementtypeused,typicalvaluesare:

Allmatlaminate:25%to35%.

Matandwovenrovinglaminate:35%to45%.

Allclothmoulding:50%.

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Table 38.3.1, Ref. [382], describes factors to be considered when selecting the wet layup process. It
detailswhatispossiblewithahandlayuptechnique.Someoftheselectionfactorsassociatedwiththe
wetlayuproutearegiveninTable38.3.2,Ref.[381].
Wetlaminationsarerarelyusedinspacestructureconfigurations.Somelaunchercomponentscanbe
appropriate, if low cost takes precedence over massefficient designs. Allcloth mouldings are
preferred because they offer acceptable massefficiency. Low numbers of complex shapes, such as
ducting,canbemadebythisprocess.

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Table38.31Wetlayupandlaminating:Troubleshootingguide
Problem

Cause

Solution
Keep mixing containers clean and free of previously catalysed gel coat. Use
throw-away mixing containers.

Cure in thickened rods or strings.

Pre-gelling.

Cracking and fissuring.

Larger cracks caused by too thick areas of gel coat or


excessive exotherm or thin point in lay-up. Fissuring
because of front or reverse impact blow.

More uniform application of gel coat and better mixing with catalyst. Prevent
accidental or injuring blows.

High exotherm, coarse weave material too close to gel


coat.

Cure laminate in steps: use lower exotherm resin. Put more mat in front of
woven roving. Best solution is application of an intermediate layer of more
rigid resin-containing Vitro-Strand fibres.

Resin too low in viscosity, resin with insufficient


thixotropic agent; mould or room too warm.

Most probable correction is to increase thixotropic agent content of resin.

Fibre pattern: random fibres from


mat or cross-hatch from woven
roving weave.
Lay-up draining on vertical
surfaces.

Drainage of resin in large lay-up to a low point and,


because of high exotherm, results in cracking: possibly
too high a resin to glass ratio.
Unbalanced laminate. Flat surface.
Under-cured in mould.

Add 0.2% green pigment to lay-up resin to see voids. Work lay-up more freely
with brushes, squeegees, or serrated rollers. If possible, apply a liberal
quantity of resin onto work before applying reinforcement, so that the resin
forces air out from the bottom.
Select more highly wettable or soluble mat or woven roving. Use loose-mixed
putty to caulk small radii curvatures prior to lay-up. Redesign mould.
Correct placement and cutting errors. Lay in patches to correct thin spots
prior to removal from mould. Try pre-wetting of reinforcement by resin prior
to placement in mould.
For finish layer, apply woven fabric, woven roving, or veil mat on inside. After
cure, sand and apply splatter paint.
Introduce more thixotropic agent into resin. Continue to squeegee excess
resin out of collection points until gelling occurs. Add additional
reinforcement.
Use symmetric lay-up. Design slight radius in surface,
Allow full cure in mould.

Hard spot.

Use fillet in corner where stiffener meets laminate.

Bubbles.

Air entrained in reinforcement after combination with


resin.

Bridging over small radius curves


such as lap-strokes, etc.

Reinforcement too stiff: curves below design-allowables.

Thin areas.

Gaps in lapping reinforcement caused by improper


placement or short-cutting, etc.

Fibres protruding from inner layup surface.

Usually unavoidable if mat is sole reinforcement.

Cracked or resin-rich areas


usually at bottom or well-point.
Warpage of part.
Distortion of part.
Cracking next to stiffening
members.
Low impact strength.

Insufficient glass: too much flexing.

Slow curing laminating resin.


Roller picks up fibres when
working on mat.

Environment changes.
Too close to gel time: styrene evaporation; rolling too
fast.

Use bag moulding, more woven roving, roving, use stiffener or sandwich
construction.
Adjust catalyst to weather changes.
Adjust gel time; adjust fans; dip roller in styrene or fresh resin; more
deliberate rolling.

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Table38.32Handwetlayup:Selectionfactors
Characteristic

Minimum inside radius


Moulded-in holes
Trimmed in mould
Undercuts (split mould)
Minimum draft recommended
Minimum practical thickness
Maximum practical thickness
Normal thickness variation
Maximum thickness build-up
Corrugated sections
Metal inserts
Limiting size factor
Metal edge stiffeners
Bosses
Fins
Hat sections
Moulded-in labels
Raised numbers
Translucency
Strength orientation
Typical reinforcement content

TypicalLimits

6.4 mm
Large
Yes
Yes
2 (0.035 rad)
0.76 mm
Virtually unlimited
0. 50 mm
As desired
Yes
Yes
Mould size
Yes
Yes
Difficult
Yes
Yes
Yes
Yes
Random or directional
25 to 65 wt. %

38.3.3

Prepreg lay-up

38.3.3.1

General

Fabricationofadvancedcompositestructuresneedstheaccurateplacementofthereinforcingfibres,
withinamatrix,inanorientationthatprovidestheengineeringpropertiesspecifiedinthedesign.
PrepregmaterialsaresuppliedinaBstagecondition,inwhichthethermosettingresinhasalevelof
tack.Thermoplasticprepregsdonothavethisinherentfeature,[Seealso:6.36forprocessingmethods
forthermoplasticbasedcomposites].

38.3.3.2

Basic processes

LayerafterlayerofUDprepregtapes,orprepregfabrics,areplacedinaprescribedorientation,by:

Directlayup,wherepliesarelaidupdirectlyonply,withoutseparatetemplates,asshownin
Figure38.3.2.

Indirectlayup,whereseparateplytemplateswithsubsequentstackingoftheplies,asshownin
Figure38.3.3.

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Itiscommonpracticetopreassemblepliesonspecialplastictemplates.Thisprocedureisperformed
inacontrolledenvironment.
Table38.3.3showsthedetailedprocessstepsforprepreglayup.

Figure38.32Prepreg:Directlayup

Figure38.33Prepreg:Indirectlayup

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Table38.33Processstepsforprepreglayup
Stage
Preparationofindividualplies

ProcessSteps
(1)AllowsealedprepregpackagetowarmtoRTbeforeopening;toavoidmoisturecondensation.

(2)Recordreel/sheet/batchnumbersasitisused.

(3)Wipeexposedtemplateswithsolventoncleanlintfreecloth,airdry.

(4)Unrollsufficientprepregforonestrip.
(5)Cuttorequiredlengthusingcleanscissorsorsharpknife.
(6)Placeprepregontemplate.
(7)Repeat(4)to(6)ensuringnogapsoccurbetweenadjacentstripswithintheply(layer).
(8)Workprepregagainsttemplatetoinsuregoodcontact.
(9)Removeseparatorstrip(backingfilm).
(10)Inspecteachplyfor:

fibredamage,

overlapsorgaps,

foreignmattercontamination.

(11)Repeat(4)to(10)forallplies.
(12)Storefinishedlayupflatinclean,moistureprooffilm.
Caution:MinimisethetimeprepregsarekeptatRT.
Preparationofmould

(1)Clean,toremoveallforeignmaterial.

(2)Polish,tocreatesmoothsurface.

(3)Solventwipeandairdry.
(4)Applyrelease(parting)agent.
(5)Applynonporouscoatedfabric,ifpartisnottobecuredincontactwithmould.

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Stage
Transferlayuptomould

ProcessSteps
(1)Applypeelply,ifrequired.(Foradhesivebondingorpainting).

(2)Aligntemplateontool,notingfibreorientation.

(3)Removeairtrappedbetweenplies,withrollerorsqueegee.
(4)Removetemplate,takingcareifprepregsareverytacky.
(5)Inspectfordamageandcontamination.
(6)Repeat(1)to(5)untilallpliesareassembled.
Caution:Documenteachplyset.

Preparationforcure

(1)Coverlayupwithperforatedreleasematerial.Donotextendoveredges.
(2)Assembleandsealboundarysupports(dams)aroundedges.

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38.4

Autoclave moulding

38.4.1

Use

Consolidationofstackedthermosettingprepregsbyautoclavecuringisthemostwidelyusedmeans
ofpreparingcompositeswithahighfibrevolumefraction.Withautoclavechambersavailableupto4
m diameter, there are few size limitations on manufacturing composite sections for satellites and
launchers.
Thecapitalinvestmentinanautoclavefacilityishighandprocessingtimesarelong.Therefore,access
to an optimumsized autoclave (from a cost perspective) can be a major criterion in a successful
project.

38.4.2

Basic process

Bstageprepregsareheatedgraduallytoinduceacontrolledresinflowandassistintheeliminationof
entrapped air and volatiles. Pressure is applied over a bag membrane to induce full consolidation
beforeresingellingoccurs.Fullcuringisachievedbymaintainingthebagunderpressureatelevated
temperature.
There are a number of variations to the basic process. These are often represented by plots of time
againstappliedpressureandtemperature.

Thepossiblevariableswithintheprocessinclude:

Debulking,

Heating(ramp)rates,

Typeofmouldmaterial,

Applicationofpositiveorvacuumpressuretothebaggedmoulding,

Dwellperiods,

Controlledbleedorzero-bleedprepregsystems,

Peel Plies,

Co-Curing,

Coolingratesandpressurerelease.

Postcuringofthelaminatedcomponentcanbeundertakenafterthepartisremovedfromthemould.

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38.4.3

Bag moulding methods

38.4.3.1

General

Bagmoulded fibre reinforced resinmatrix composites and bonded structures can comply with the
differentstandardsofqualityfordifferentdesigncriteria.Thebagmouldingprocesscanbeadapted
andoptimisedtoproducecompositeswhichperformadequately,andcompetewithalternativetypes
ofconstruction.
Innovativeadaptationsofbagmouldingprocessesareoftenmadetocreatesingle,complex,composite
structures,ratherthanseveralseparatepartswhichthenneedjoiningtogether,i.e.reducedpartcount.

38.4.3.2

Autoclave process

A prepreg stack, with all of the necessary release layers, is draped over a mould. A polymer
membraneisthensealedtothemouldsurface,awayfromtheprepreg,toformthebag.
In the autoclave chamber, the bag is placed under vacuum, so that the bag and prepreg are pulled
downagainstthemouldsurface.Positiveexternalpressureisappliedtothemouldingbypressurising
theautoclavechamber.Theadvantageofanautoclaveistheabilitytoapplya0.69MPaorabout6bar
(100 psi) positive pressure to augment the 0.1 MPa (15 psi) from the vacuum. This enables low
voidage composites to be made from high fibre volume fraction prepregs, without the need for
matcheddie,pressuretooling.

38.4.3.3

Modified processes

Bag moulding can be modified to enable a positive pressure to be applied during consolidation
withoutuseofanautoclave.Someoftheprocessmodificationsinclude:

Mouldingwithoutanadditionalexternalpressure,i.e.withonlythe1bar(15psi)atmospheric
pressure from the vacuum as the consolidating force. This relies on good resin flow and bled
prepregstoensuretheeliminationofvoidage.Fibrevolumefractionscanbelowerthanbyfull
pressureconsolidation.

Usingthemouldaspartofthepressurecontainment,or

Modifyingaplatenpresstoenablegaspressurisation.

Thevariousprocessesillustratedare:

VacuumbaginFigure 38.4.1,Ref.[382].

PressurebaginFigure 38.4.2andFigure 38.4.3forpressmodifications,Ref.[382].

AutoclavemouldinginFigure 38.4.4,Ref.[382].

InFigure38.4.1andFigure38.4.4,thearrangementsshownareforpreparingflatlaminates.
Forcomplexshapesproducedbythesemethods,theuseofrigidcaulplatesisoftennotfeasible.

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Figure38.41Vacuumbagmouldingmethod,withverticalbleeder

Figure38.42Pressurebagmoulding

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Figure38.43Pressurebagmoulding:Pressmodifications

Figure38.44Autoclavemouldingmethod,withverticalbleeder

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38.4.4

Features of bag moulding

38.4.4.1

Bags

Bags are thin, flexible membranes or silicone rubber shapes, which separate the lay up from the
pressurising gases during the composite cure. Consolidation and densification of the layup is
achievedbytheresultingpressuredifferentialsacrossthebagcontents.Thevarioustypesare:

Vacuum bags: Consolidation and densification of vacuum bag mouldings can be achieved by
atmospheric pressure alone as the bagged lay ups are evacuated during the cure cycles.
Vacuumbagmouldingistheleastlimitedastothesizewhichcanbeprocessed.

Pressure bags: Pressure baggedandautoclave cured composites are pressurised by hot gases.
Ventstotheatmosphere,orvacuum,providefortheescapeofvolatilereactionbyproductsand
theentrappedairfromthecuringcomposites.

Autoclavebags:Thebaggedlayupsinautoclavesareusuallyventedtoapressurelowerthan
thatappliedtothebag.
NOTE

38.4.4.2

Thesearesimilartopressurebags.

Consolidation

Consolidation is achieved when the separate prepreg plies within the lay ups, together with other
adherends(ifpresent),arebondedtogether.

38.4.4.3

Densification

Densificationresultsindiminutionofvoids,andremovalofexcessresin,ifappropriate.

38.4.4.4

Cure

Although vacuum bag moulded composites can be cured at room temperature, most are cured at
elevatedtemperaturestoimprovetheproperties.Thetypesofcurecanbegroupedas:

Thermal cures: These are best attained in circulating air ovens, but can be achieved using
infraredheatedorpassiveconvectionovens.

Alternativecuringmethods,[Seealso:38.12]:

Induction,

Dielectric,

Microwave,

Xenonflash,

Ultraviolet,

Electronbeam,and

Gammaradiation.

38.4.4.5

Other features

Duringcure,thevariousbagmouldingmethods:

Preventblisteringinthecomposites,

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Controlpressureandheatapplication,and

Controltheratiooffibretoresin.

38.4.5

Bagging techniques

38.4.5.1

Debulking

Debulking reduces the possibility of porosity in critical areas. It can be necessary when preparing
prepreg stacks with a large number of individual plies, or when complex shapes are involved. The
process involves placing some of the uncured plies in the mould and forming them to the mould
surfaceusingavacuumbag.Thebagisthenremovedandfurtherpliesaddedtothemouldstack.If
necessary,itisrepeatedseveraltimesespeciallyforthicklaminates.

38.4.5.2

Vacuum bag moulding

The bags form a membrane enabling the air to be evacuated from the laminate and to generate the
atmosphericpressurenecessaryforcompactionagainstthemould.

38.4.5.3

Autoclave bag moulding

The bags serve to apply the compacting gas pressure to the construction during the cure. The
atmospherewithinthebagisventedtoalowerpressuretoenableremovaloftrappedairandreaction
products.

38.4.5.4

Zero-bleed and bleed systems

Theneedforableedsystemdependsontheprepregresinformulation,where:

Zerobleedprepregsystemshavegainedwideracceptanceasameansofproducingcomposites
withpredeterminedfibrevolumefractions.Theseprepregshaveresinswithoptimisedviscosity
andgelationcharacteristicstoavoidexcessiveresinflowtoeliminatevoidage.

Controlledbleedprepregsremainandareusedasameansofassistingconsolidation.

Bleedoutsystemsaredesignedtomaintainthereducedpressureswithinthebag.Ifthisisnotdone,
gaspressurewithinthebagpreventsconsolidation.
Thecorrectapplicationofpressureachieves:

Consolidationofthesuccessiveplies,

Completionoftheresinimpregnationofthefibre,

Eliminationof:

voidcreatingvolatiles,

reactionbyproducts,and

entrappedair.

reductionoftheexcessresininthelayup.

Thebaggedlayupincludesthebleedoffsystemdesignedforthecompositepart.Baggedlayupscan
beverticallyoredgebled.

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Theclassicaldifferencesbetweenthetwoareillustratedfor:

Verticalbleed,[See:Figure38.4.4].

EdgebleedinFigure38.4.5,Ref.[382].

Verticalbleedisusuallymoreefficientthanedgebleed.

Figure38.45Bagmoulding:Edgebleedoutsystem

38.4.6

Tool materials

38.4.6.1

General

Variousmouldortoolingmaterialsareused,notablysteel,aluminium,compositesandInvar.
Eachhasitsownmeritsandthechoiceisusuallyinfluencedbyacombinationofthe:

Mouldcost,e.g.material,shape,precision.

Thermalconductivity,

Thermalexpansion:matchingCTE(toolmaterial)withCTE(mouldingmaterial),

Durability(reuse).

The merits of various tool materials are shown in Table 38.4.1. The comments apply to CFRP
mouldings.

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Table38.41Toolingforcomposites:RelativemeritsofvarioustypesforCFRP
Factor

Steel

Aluminium

CFRP

Invar

Cost

Low

Medium

High

Thermal
Conductivity
Thermal
Expansivity
Mould mass
Durability

Medium

High

Medium/Hig
h
Medium/Low

Medium

Medium

High

Low

Low

High
Good

Medium
Reasonable

Low
Reasonable

High
Reasonable

38.4.6.2

Steel

Steel moulds are used because it is a lowcost material, easily machined and durable. For
manufacturingaccuratelydimensionedCFRPcomponents,theCTEdifferencebetweensteel(+15x10
6/C)andCFRP(from1to+3x106/C)canbetoogreat.Steelexpandsappreciablyduringheatingto
thecuretemperatureandthencontracttoagreaterextentthanthemouldingoncooling.

38.4.6.3

Aluminium

Aluminium has good thermal conductivity, which assists in obtaining an even temperature
distribution. However, its thermal expansion is very high (+23 x 106 /C). It is also more easily
damagedthansteelandcansufferthermaldistortionwithrepeatedheatingandcoolingupto180C;a
typicalprocessingtemperatureforthermosettingCFRP.

38.4.6.4

Composite (CFRP)

By using CFRP for the mould tool, a close CTE match can be achieved with the moulding.
Consequently,thedimensionsofthemouldchangelittleduringtheprocessingcycle.AsCFRPtools
cannotbemachinedfromstockmaterial,theyaremouldedfromamaster.Thisinturnisachievedby
machining a replica of the final component surface and preparing a mould from it. The replica is
usually steel or machinable ceramic. The tool can be made using low temperature curing epoxy
prepreg,whichispostcuredtogiveatoolingCFRPwithahighglasstransitiontemperature.CFRP
toolingshouldbecarefullystoredandhandledtopreventdistortionordamage.Thereisoftenalimit
onthenumberofelevatedtemperaturemouldingswhichcanbetakenfromasingleCFRPtool.

38.4.6.5

Invar

TheCTEofInvaris0.9x106/C,whichissimilartothatofCFRPcomponents.Thehighmaterialcost
andlowthermalconductivitydetractfromitswidescaleusage.

38.4.6.6

Other tool materials

Othermaterialsareoccasionallyused,including:

Graphite

Castceramic

Thesecanbeeasilyshapedbutarenotparticularlydurable.Theycanbeusedforprototypemoulds.

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38.4.7

Cure schedules

AtypicalcurescheduleforthemouldingofthermosettingCFRPisgiveninFigure38.4.6.
Cure schedules are usually recommended by prepreg manufacturers, based on the preparation of
simple,flatlaminates.
For complexshaped mouldings, it can be necessary to modify the recommended cure schedule to
produceacceptablequalitylaminates.Thiscanbeachievedthroughexperienceofaparticularprepreg
orbyevaluationstudiesforanewprepregsystem.
The critical aspect of any cure schedule is the total time. This is determined by establishing the
optimumconditionsforconsolidatingtheprepregtoproducevoidfreecompositesofthecorrectfibre
volumefraction.Thetotalcurecyclecannotbetoolongortooshort.

Comments:

Forpressuredcurecycleapplypressurefromstart.

Forvacuumcuredthicksections(>3.2mm),insertionofa60minutedwellat100Cis
recommended.

Figure38.46Typicalcurescheduleforautoclavedprepregs

Featuresofthecurescheduleare:

Temperatureramprate,usuallyvariesbetween1and6C/min.Itisdeterminedbythe:

gelcharacteristicsoftheresin,

resinviscosity(zerobleedorcontrolledbleedsystems),

thermalinertiaoftheautoclave,assembledtoolingandmoulding.

Dwell periods, which are used to eliminate voidage by enabling resin flow prior to gelation.
Thereisanincentivetoreduceoravoiddwellperiodsinordertoreducethetotalelapsedtime.

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Time at maximum temperature, which is determined by the extent of curing (crosslinking);


typicallyfrom2hoursto4hours.

Cooldownrate,whichislargelydictatedbyhowquicklytheautoclaveandtoolingassembly
canbecooledtothepointwherehandlingthemouldingispossible,takingintoaccountthat:

unevencoolingofamouldingiscancausedistortion.

vacuum is maintained on the moulding during cooling and possibly some positive
overpressureonthebag.

Although reducing the maximum temperature in the autoclave can reduce residual stresses in the
curedmoulding,itoftenresultsinanextendedcurecycleinordertoobtainthesamecrosslinkdensity
inthecuredresin.

38.5

Filament winding

38.5.1

Basic process

Filament winding was one of the earliest techniques used to produce composite materialstructures.
This process uses continuous strands of glass, carbon or aramid fibres which are continuously
impregnatedwithalowflowresin.Thestrandsarethenwoundontoamandrel,whichprovidesthe
finalgeometry.

38.5.2

Applications

Variousstructurescanbefabricatedusingthistechnique,including:

Cylindricaltubes;themostcommonapplication,Ref.[384].

Containersforfluids,gasesorsolids.Thesecanhaveopeningsattheirpoles.

Flatpanels,byfirstwindingonamandrel,thencuttingthefinishedlayupalongthelengthof
themandrel,flatteningandcuringunderpressure.

Geodesiclatticestructures.

Filamentwindingprovidesanefficientmeansofobtainingoptimisedpressurevesselstructures,[See
also:Chapter29].
Dependingontheappliedloads,weightsavingscanbeobtainedbychangesto:

fibreangle,or

thicknessoflayup.

Modernwindingmachines,knownaswindingrobots,canproduceverycomplexgeometrypartsby
usingnonlinearwindingprograms.

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38.5.3

Winding process

Themainprocessstepsconsistof:

Fibrepreparation:Afterthechoiceoftheappropriatefibre,giventhedefinedrequirementsfor
thestructure,fibrebatchesare:

dried,inanovenatabout130Cforseveralhours.

stored,at60Cforsomedays.

Fibreimpregnation,bycontinuouslypullingfibresthroughabathofresin,asshowninFigure
38.5.1. To control the resin content, the impregnated fibres are squeezed through a pair of
rollers.

Tensioning:Theimpregnatedstrandpassesthroughrollerstoprovideacertainpretensionin
thefibre.

Strandguidance:Thestrandsarepassedthroughaguide,andthentothemandrel.

Winding,ofthestructure.

Precure:Thefinalfilamentwoundstructureisthenheatedbyinfraredlighttoabout80Cin
ordertoprecuretheresin.

Finalcure:Afterprecure,thestructureisplacedinanautoclavetoperformthefinalcuringat
normally130Cforseveralhours.Thecuretemperaturedependsontheparticularresinsystem.

Removemandrel:Dependingonthetype,[Seealso:Mandrels]:

Reusableareextractedfromthestructure,or

Lostarebrokenandremoved.

Postcure,ifnecessary.

Figure38.51Filamentwinding:Impregnationoffibres

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38.5.4

Mandrels

38.5.4.1

General

Geometry and quality of the inner surface of the filamentwound structure depend on the material
andonthesurfaceofthemandrelused.Factorstobeconsideredinclude:

extraction,

material,

surfacepreparation,and

componentshrinkage.

38.5.4.2

Reusable

For wound tubes,a mandrel of polished or chromeplated steel is commonlyused. Other materials,
e.g. aluminium, need more effort concerning release agents. A collapsing mandrel is another
possibilitytoenableitsreleasefromthestructure.

38.5.4.3

Lost

Forspheres,ellipsoidorcylindricalcontainershavingawoundend,normallylostmandrelsareused.
Thesecanbemadefrom:

Sandinasolublebinder,

Gypsum,

Foam,or

Lowmeltingpointmaterials.

Thesemandrelsneedafinalsurfacetreatmenttoprovidegoodrelease.

38.5.4.4

Integral

Forapplicationsthatneedaninnerlinertopreventleakageordamagetothecompositestructure,e.g.
pressure vessels. The mandrel can form part of the finished structure. This is also called over
wrapping,i.e.wherethelinerisusedasthemandrel.

38.5.4.5

Component shrinkage

Mostresinsystems,andthereforethereinforcedstructures,tendtoshrinkaftercuring.Thiscanmake
themandreldifficulttoremove.Amandrelwithahighercoefficientofthermalexpansion,relativeto
thecompositestructure,canbeheatedduringthewindingsothatoncoolingdownitcontractsaway
fromthecomponent,soaidingitsremoval.

38.5.5

Sandwich constructions

It is feasible to filament wind sandwich constructions. Cylindrical constructions have been


manufacturedbydirectlywindingontohoneycombmaterial,[Seealso:29.12].
Forcylinders,thesequenceusedcanbe:

Windingofinnerskinontomandrel,

Bondingofhoneycombcoreontoinnerskin,

Overwindingouterskintocompletethecylinder.

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38.5.6

Tape winding

Narrow, continuous widths of Bstage prepreg can be used instead of fibres wetted with uncured
resin. The width of prepreg tape is limited when winding complex shapes to ensure that the fibres
conform to the mould in an acceptable manner. This route is suited to winding cylinders, but not
necessarilyfordirectwindingontohoneycombcorematerial.
Tapewindingisalsoapplicabletothermoplastics,Ref.[386].
[Seealso:6.26]

38.6

Filament-winding machines

38.6.1

General

Machines,designedtoperformwindingprocesses,arecommonlyeither:

polarplanar,or

helical.

Allmachinesareavailableinseveralvariants,whichaddversatilityandcompensatesforsomeoftheir
weaknesses.
The development of computercontrolled, filamentwinding robots has made complex winding
patternsforlargestructuresfeasible,[See:29.2].

38.6.2

Polar winding

Polar machines are generally used for the production of containers with diametertolength ratios
greaterthan0.5.

Vertical mandrel: Polar winding machines normally have the mandrel mounted in a vertical
position, which enables a simpler construction of the rotating arm because deflection of the
mandreliseliminated;asshowninFigure38.6.1.Thisarrangementislimitedtostructuresof
moderatesize.

Horizontalmandrel:Forlargewindings,themandrelissupportedinahorizontalpositionand
therotatingthreadguideplacesthefibresonthemandrel,asshowninFigure38.6.2.

Tumbler:Avariationofthenormalpolarwindingsystemisthetumblingprocessinwhichthe
thread guide remains stationary while the mandrel rotates or tumbles in a near horizontal
plane,asshowninFigure38.63.Theinclinationofthemandreltothehorizontaldeterminesthe
windingangle.

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Figure38.61Filamentwinding:Polarvertical

Figure38.62Filamentwinding:Polarhorizontal

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Figure38.63Filamentwinding:Polartumbling

38.6.3

Helical winding

Helicalwindingmachinesconsistofarotatingmandrelandareciprocatingthreadguidancecarrier,as
showninFigure38.6.4.
Inadditionathirdmotionperpendiculartothemandrelaxisisappliedtoimprovethefibreplacement
overtheenddomes.
To achieve optimum placement of the fibres on a geodesic path, sophisticated control of the thread
guidanceisnecessary.Thewindingangleisdeterminedbytheratioofmandrelrotationtothespeed
ofthethreadcarrier.

Figure38.64Filamentwinding:Helical

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38.7

Resin transfer moulding

38.7.1

General

Resintransfermoulding,RTM,isalowercostcomponentproductionprocessthanprepreglayupand
autoclavecuring.CertaincomplexshapescanbemorereadilymadebyRTMthanbyothermoulding
routes,Ref.[387],[388].

38.7.2

Basic process

A fibre preform, formed to the intended component shape, is placed in a matched mould, which is
thenclosed.Alowviscosityresinisinjectedintothemouldandallthefibreswettedthroughuntilthe
mould is filled. The resin is injected under pressures of about 0.69MPa (100 psi), with or without
vacuum assistance in the mould cavity. A heated curing cycle is applied. The cure conditions are
dependentontheresinused.
ThesimilaritiesbetweenRTMandresininjectionmoulding,RIM,canmakeitdifficulttodistinguish
betweenthem.
TheRTMprocessisasimpleconcept,asshowninFigure38.7.1.However,theprocessingparameters
shouldbecarefullycontrolledtoensurehighqualitynetshapecomponents.
Proprietary technology packages are becoming available which match the resin and fibre preform
technology.AnexampleistheInjectexsystemfromBrochierCibaGeigy.

Figure38.71Resintransfermoulding(RTM):Process

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38.7.3

Applications

Within industry generally, RTM is applied where the component production numbers are high;
typically measured in hundreds or thousands per year. This is not normally the case with space
structure manufacturing which rarely exceeds ten units in total, except for launchers, e.g. Ariane
series,orforelementsinlatticestructures.
The attraction of the process for space applications is closely linked with the need for complicated
componentshapes,i.e.thosewhichcannotbereadilyproducedbyothercompositemouldingroutes.
Someexamplesofsuchcomponentsinclude:

nosecones,

radomes,

integrallystiffenedpanels,

complexshapedducting,

CFRPadapterrings;asforArianelaunchers,Ref.[389],

J,T,C,andIstructuralshapes,Ref.[3810],

braidedringsandtubes,Ref.[3811],

nozzlecomponents,Ref.[3812].

RTMismostpracticalforthicknessesintherangeof2mmto12mmandnotforverythinsections.
Tolerances on wall thickness depend on the accuracy and stiffness of the mould tooling. Typically
wallthicknesscanhaveatoleranceof0.25mm.Fibrevolumefractionsareusuallyslightlylowerthan
thoseachievedwithpressureconsolidatedprepregs.
Polymer composite mouldings made by RTM are used for preparing hightemperature composites.
Using pyrolysis, the moulding (green part) can be converted to carboncarbon or SiCbased
constructions. These preforms are subsequently densified by further infiltration methods, e.g. CVD,
CVIorfurtherresinadditions.
[See:Chapter88formanufacturingtechniquesusedforhightemperaturecompositecomponents]

38.7.4

Fibre preforms

38.7.4.1

General

The development of versatile and costeffective fibre placement technology is central to RTM
manufacturingasachievehighproductivity.
Theuseofmachinerytocreateanetshapepreformwithallthefibresinthedesiredorientationsand
quantitiesisessentialtoavoidcostlymanuallabour.Preformscanbeproducedfrom:

Wovenfabrics,

Tubularorflatbraiding,

Stitchedlayers,

Multidirectionalweavings,

Knittedsections.

Fibre volume fractions can be varied between 30%and 70% by volume, but50 volume % is typical.
Bothcarbonandglassfibresareused.

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38.7.4.2

Binders

A polymeric binder is often used to hold the preform together. Such binders have to be compatible
withthematrixresinandassistresinimpregnation.

38.7.4.3

Cores

Foamcorescanbeincorporatedwiththefibrepreformtoprovidesupportforthinwallconstructions.

38.7.5

Resin injection

38.7.5.1

General

Anewgenerationofthermosettingresinsareformulatedspecificallywithoptimumviscosityandcure
characteristicsforRTMprocessing.Theseinclude:

Epoxies,

Bismaleimides,

Others,including:cyanateesters,phenolicsandsilicones.

38.7.5.2

Epoxies

ExamplesofepoxyresinsformulatedforRTMprocessinginclude:

ShellRSL1895/W,Ref.[3813],[3814]andDPL862/RSC763(twopartliquidepoxies),

ShellEpon9400/9450and9405/9470,Ref.[3811],

HerculesHBRF311andHBRF314,

3MPR500(hotmelt),

DowPlasticDER300(hotmelt)andTactix123,

BPE905L,Ref.[3814],

CibaGeigyXUMY722/RD91103,Ref.[3815].

38.7.5.3

Bismaleimides

ExamplesofbismaleimideresinsformulatedforRTMprocessinginclude:

X20644(DowUnitedTechnologies)basedonBASF52504prepregresin(hotmelt),

ModifiedMatrimid5292(CibaGeigy),Ref.[3816],

Compimide65FWR(Technochemie/Shell),Ref.[3817],

XNF650(Hexcel).

38.7.5.4

Others

OtherchemicalgroupsofresinsforRTMprocessinginclude:

Cyanateesters,e.g.DowXU71787,Ref.[3818],[Seealso:6.35].

Phenolics,Ref.[3812],

Silicones,Ref.[3812].

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38.7.6

Process variables

38.7.6.1

General

Theprocessvariablescanbesummarisedas,Ref.[3819]:

Resinviscosity(initially25cpsto50cps)dependingon:

temperature,

potlife.

Dryfibrepreformandbinderhavetobewettablebyliquidresin,e.g.Injectexsystem.

Applicationofpressureandvacuumtocontrolresininfiltration.

Positionandnumberofinletandoutletports.

Initialdegassingofresin.

Evacuationofairfrompreform.

Toolingmaterialformatchedmaleandfemalemouldparts.

Mouldclampingandsealing.

Mouldtemperatureandpostcure.

38.7.6.2

Resins

The resin can be either a onepart system (hotmelt, similar to prepreg formulation) or twopart
(liquids mixed at the point of use). Onepart systems are normally used for aerospace components,
Ref.[3820],becausethisenables:

greaterconfidenceinchemicalcompositionfromtheresinsystemsupplier,

similarcuredresinperformancetothatachievablebyprepregs,

roomtemperaturestorageforupto6months.

38.7.6.3

Resin flow modelling

Forsuccessfulmouldings,theflowofresinintothemouldcavityandpreformshouldbeoptimised,
Ref.[3821],[3822].Problemstoavoidare:

Gellingoftheresinbeforethepreformiscompletelyfilled.

Incompleteresinflow,leavingtrappedairandhencevoidage.

Suchdefectsarelimited,largelybytrialanderror,ifalargeproductionrunisanticipated.Forvery
limited unit production numbers, the process needs to be optimised at the planning stage to avoid
unsuccessful prototypes. Consequently, computeraided design tools are often used to model the
process,Ref.[3821].

38.7.7

Process advantages

TheindividualprocessadvantagesofRTMarenotnecessarilyunique.Buttakenasawhole,RTMcan
beappropriateforsomecomponentdesigns.ThecharacteristicsofRTMinclude:

Preformsenablemultidirectionalreinforcementplacementtoimprovedamagetolerance.

Goodsurfacedetailandaccuracy.

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Complexshapes,withintegralstiffening,canbemadeinasinglemoulding.

Nearnetshapepartsneedingminimummachining.

Reinforcementlayupisdryinsteadoftackyprepreg.

Refrigeratedshippingandstorageisnotalwaysnecessary.

Closeprocesscontrolcanreducetheneedfornondestructiveinspection.

Sectionshavingvariablethicknessarepossible.

Totalprocesstimesarereducedcomparedwithautoclaving.

38.8

Pultrusion

38.8.1

Use

Pultrusion is a wellestablished, industrial manufacturing process for both thermoset and


thermoplastic composites. It is similar to the extrusion of metal alloys and plastics. The process is
ideally suited to the continuous manufacturing of constant crosssection profiles, in hundreds or
thousands of metres (total). There are, however, few space applications which consume such large
quantitiesofpultrusioninasingle,standardsize.Theprocesscanbeusefulforapplications,suchas:

Tubesforlargelatticestructures,

Profilesforconstantsectionribstiffeners,

Ducting,whereofftheshelfpultrudedsectionsaresuitable.

Continuous sections up to 1m wide can be made by pultrusion, including integral stiffeners and
doubleskinconstructions.
Intheearly1980s,NASAexaminedthepossibilityofusinganinorbitpultrusionfacilitytoproduce
thermoplastic composite sections in space rather than transporting formed lengths from Earth. The
sectionswerethentohavebeenassembledtoformthemainstructuralelementsofaspacestation.

38.8.2

Basic process

38.8.2.1

Thermosetting resins

ThebasicprocessisshowndiagrammaticallyinFigure38.8.1.Theprocessstepsare:

Spoolsoffibres(sufficientfortheproductionrun)arepurchasedandarrangedtomakeupthe
necessaryfibrefractioninthefinalcompositesection.

Fibretowsaregatheredanddrawnthrougharesinbathandimpregnated.

Impregnated fibres are continuously drawn (maximum 1m/min) through a heated die of the
desiredcrosssectiontoshapethecomposite.

Alongdieisused,whichincorporatesappropriateheatingelements.

Thetotalelapsedtimewithintheheateddieregionissufficienttofullycuretheresin.

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NOTE

Selection of the resin is important in determining the production


rate.

Hauloffequipmenttakesthefinishedproductawayfromthedie,andthepultrusioniscutto
specifiedormanageablelengths.

Figure38.81Pultrusion:Basicprocess

Thestartupcostscanbehigh,becauseofthe:

Complexheated,shapeddie,and

Procuring sufficient spools of fibre for the crosssectional area of pultrusion to be made; cost
dependsonthetypeofcarbonfibresspecified.

38.8.3

Pull-forming

38.8.3.1

General

Thisisamodifiedpultrusionprocessincorporatingdirectshapemoulding.

38.8.3.2

Process

Fibre and resin are combined by drawing them through a shaped die to the desired length. That
length is then enclosed in a mould and formed to the final shape by application of direct heat and
pressure.Thefibresarecutasthemouldcloses.Thismethodenableschangesinsectiontobemadein
themoulding.Ahighdegreeofautomationisretainedbecausethecontinuousdrawingprocesscan
beoperatedusinganumberofmoulds.

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38.9

Table rolling

38.9.1

Tubular sections

Tablerollingcanbeusedforproducingfinitelengthsofcylindricalorfinetaperedtubularsections.
Theprocesscanbeappliedto:

unidirectionalthermosettingfibreprepregsforsmalldiametersections,

fabricprepregsforlargerdiameters.

Prepregisrolledontoasteelmandrelformerandbaggedforautoclavemoulding.Theprocessneeds
careful control to prevent ply rucking on small diameter sections. This can occur during the
consolidationastherolledprepregcompactstothefinaldiameter.
Thewallthicknessofthesectionsproducedcanvarybecausetheprepregendsareoverlapped.

38.10

Pressure and mechanical forming

38.10.1 General
Consolidated laminates of some typesof compositematerials can be shaped by plastic deformation,
i.e.pressureormechanicalforming.Thematerialsthiscanbeappliedtoare:

FMLfibremetallaminates,[See:46.1.5formaterials]

Thermoplasticmatrixcomposites,[See:6.26].

Variationsofthebasicpressureformingtechniqueareusedforthesemaintypesofmaterials.
Theamountofplasticdeformationisrestrictedbythe:

Limitedretentionoflaminateintegrity.

Controlofreductioninthickness.

Shapecomplexity,i.e.multiplecurvaturesanddeeprecesses.

38.10.2 Fibre metal laminates


ARALL, GLARE and CARE are FML materials, [See: 46.17]. These are hybrid laminates
containingmetalandthermosetcomposite.FMLcanbeformedasiftheywereductilemetalsheets.
Appropriateprocesstechniquesinclude:

Rollforming,

Brakepressbending,

Rubberbackedbending,

Stretchforming,and

Rubberpadforming.

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38.10.3 Thermoplastic composites


38.10.3.1 Continuous fibre-reinforced composites
Theprocessingoptionsinclude:

Pressclaving,

Diaphragmmoulding,

Hotorcoldforming,and

Deepdrawing.

[See:6.26forprocessdescriptions]

Diaphragm moulding, in conjunction with a modified autoclave, has produced parts with complex
curvatures,Ref.[3823].Forexample:PEEKAPC2aircraftspoilersections,upto2.2mlong,havebeen
madewithin20minutes.

[Seealso:38.11formouldingofshortfibrereinforcedthermoplasticcomposites]

38.11

Injection moulding

38.11.1 General
Injection moulded is usually associated with the highvolume manufacture of industrial and
consumer products, i.e. large number of identical parts. Occasionally, injectionmoulded,
thermoplastic components are used in space applications, but the high mould costs need to be
justified. It can be feasible for small attachments, where other composite processing routes are not
practical.

38.11.2 Short fibre composites


38.11.2.1 General
For massefficient designs, glass or carbon fibrereinforced polymers are preferred. These contain
about 30% of reinforcement phase in order to provide adequate stiffness. The matrix is normally a
highperformanceengineeringthermoplastic,suchasPEEK,PEIorliquidcrystalpolymers,LCP,Ref.
[3824].

[See:6.17forfurtherinformationonthermoplasticmatrices]

38.11.2.2 Complex shapes


GlassfibrereinforcedLCPliquidcrystalpolymercomponentshavebeenusedinaspaceprogramme
wheregoodthermalinsulationpropertieswereneeded,Ref.[388].

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Theitemstargetedforinjectionmouldingwere:

Highflowlatchbracket,

Cantileverpipesupport,

Pyrovalve,

Pressuretransducer,

Fillanddrainvalve,

Pipesupport,and

Liquidfilter.

38.12

Radiation curing

38.12.1 Process developments


38.12.1.1 General
Ionisingradiation,suchasEBelectronbeam,XrayorGammarayaremostlyusedfor:

Sterilisationoffoodormedicaldevices,

Crosslinkingofthermoplasticbasedmaterial,

Dryingofcoatingsandinks.

38.12.1.2 Composites
Theuseofheatinelevatedtemperatureprocessesistheacceptedmethodforcrosslinking(curing)of
thermosettingresinformulations.
Withtheoverallaimofimprovingprocessefficiency,thereisanincreasinginterestinusingdifferent
formsofelectromagneticenergyinordertoobtaincrosslinking,Ref.[3825]to[3834].
Resinsareformulatedtobereceptivetoradiationenergyandsoachieveefficientcrosslinking.
Using energy sources, other than heat, within industrial processes for composites is a fairly recent
innovation,soequipmentwithaprovencapabilityisuncommon.
Thebroadcategoriesofradiationappliedtocompositeresincuringare:

Electronbeam,EB.

Microwave.

Ultravioletlight,UV.

38.12.1.3 Potential benefits


Thepossiblebenefitsofusingelectromagneticradiationcuringcomparedwithconventionalthermal
processinginclude:

Reducedprocesstimes,i.e.rapidcure,

Reducedenergyconsumption,

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Lowerprocesstemperatures,

Reducedinternalstressesinthecuredcomposite,

Improvedpolymerisation,

Reducedretentionofvolatiles.

38.12.2 EB electron beam curing


38.12.2.1 Thermosetting resins
Use of EBcuring for composite materials is still limited. However, the technology offers numerous
significantadvantagesoverconventionalheatcuringprocesses,including:

EBtechniquesofferthecapabilityofcuringverylargestructuresoutofautoclave,usinglow
energybeamscoupledwithwindingmachines.

Complexshapesandassembliescanbeprocessedeasily

Thermalgradientsinthickcompositepartsaremoremanageable.

Toolingislessexpensiveduetothelowertemperaturesthattheyexperience.

Shelflifeofmostcurableformulationsisveryadvantageous.

VOCemissionsarereduced.

Processingtimesareshorter.

Energycostsarereduced.

38.12.2.2 EB-curing resin formulations


The interaction of ionising radiation with the precursor materials creates initiation sites for the
subsequentchemicalreactions.Thenatureofthesereactionsdependonthepreciseformulationofthe
resin.Ingeneral,threetypespredominate,i.e.:

Polymerisation,

Crosslinking,

Materialdegradationbychainscission.

In the case of formulations with radiationsensitive components (monomers or prepolymers), the


interactions can lead to rapid polymerisation. The reactive resins can be broadly grouped by their
polymerisationmode:

Radical:mainly(meth)acrylatebasedformulations,

Cationic:epoxyresins.

TypicaladvantagesanddrawbacksofbothsystemsaresummarisedinTable38.12.1.

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Table38.121EBcuring:Advantagesanddrawbacksofepoxyandacrylateresins
CharacteristicsofEBcuringformulations,bypolymerisationmode
Process
stage

Freeradical(Acrylates)

Advantages

Cationic(Epoxy)

Drawbacks

Advantages

Drawbacks
Poor initiator
compatibility
Low stability

Pre-cure
propertie
s

Low cost
chemicals
Shelf
stability

Compatibility
with
thermoplastic
additives

During
cure

No initiator
needed
Easier
control of the
reaction

Sensitivity to
oxygen
High volume
contraction

Insensitivity to
oxygen
Low volume
contraction

Sensitivity to
bases and
nucleophiles
(water)

Brittleness
Current carbon
sizing not
adapted

No termination

Post-cure
propertie
s

Thecuringmechanisms,theinfluenceofformulation,dose,doserate,doseapplicationsequenceand
temperatureonthecuringprocess,reactionkineticsandnetworkpropertiesarewellknown,Ref.[38
40].
Forsomeacrylatebasedsystems,thepolymerisationrateisproportionaltothesquarerootofthedose
rateattheverybeginningofthepolymerisation.Theterminationreactionisbimolecular,i.e.reaction
oftworadicals,atpolymerisationfromtheliquidtogelstate.Then,thereactionisdiffusioncontrolled
withthereactionrateproportionaltothedoserate.Temperaturethusinfluencesboththereactionrate
andtheultimatecuringlevel.
The dose and dose rate application in large composite structures can be modelled, as well as the
reactionkinetics.Hence,thepropertiesofthecompositematerialsintermsofextentofcuringcanbe
accurately predicted with regard to the processing conditions. Consequently, the process is
predictable,controllableandreliableforindustrialapplications,Ref.[3841],[3842].
AgeingofEBcuredcompositestructureshasalsobeenstudiedandnoparticularsensitivityoftheEB
cured systems was observed. The toughness of EBcured formulations has been improved and is
similar to that of heatcuring resin systems. The mechanical performance of the materials has
increasedand is suitablefor very highperformance applications, Ref. [3843],[3844], [3845]. When
agedinwater,EBcuredresinshavethesamebehaviourasheatcuredresinsystems.
SometypicalmatricesbeingusedforEBcuringarepresentedinTable38.12.2.

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Table38.122EBcuring:Mechanicalpropertiesofsomeacrylateandepoxyresins
Resinsystem

Fracturetoughness(1)K1C
(MPa.m1/2)

Glasstransitiontemperature(2)Tg
(tan)C

0.6
0.6
1.5

170
210
140

0.9

205

Acrylate:
EP-AC
EAR2
EB600-BPaPx
Epoxy:
CR2 (epoxy)
Key:

(1)FracturetoughnessmeasuredaccordingtostandardIGC0426680;
(2)GlasstransitiontemperaturesmeasuredbyDMA,resonantmode,5C/min

38.12.2.3 Properties
PropertiesofEBcuredunidirectionalcompositearegiveninTable38.12.3.

Table38.123EBcuring:TypicalmechanicalpropertiesofunidirectionalIM
carbonfibre/acrylateresin
IMcarbonfibre/EPACacrylateresin
UDproperties,at23C

(65%fibrevolumefraction)

Tg (C )
Longitudinal tensile properties:
Strength (MPa)
Youngs modulus (GPa)
Longitudinal compression
properties:
Strength (MPa)
Youngs modulus (GPa)
Longitudinal bending properties:
Strength (MPa)
Youngs modulus (GPa)
Interlaminar shear properties:
Strength (MPa)

170
2600
174
1000
141
1600
150
80

ThefirstgenerationofEBcuredcompositesshowedthatthegenericmechanicalpropertiesarevery
similartothefirstgenerationofheatcuredepoxyresinsusedforaeronauticapplications.
Themajorweaknessescomparedwithnewercompositeswithtoughresins,suchasIM7/9772,arethe
lowerinterlaminarandtransversetensilestrengths.

38.12.2.4 Demonstration parts and structures


Severallarge,demonstrationpartsandstructureshavebeenmanufacturedusingEBtechnologies;as
illustrated in Figure 38.12.1. The items shown are fullscale components cured by electron beam
processingusinga10MeVelectronbeam.

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Large wound carbon fibre


composite vessel

Resin characteristics:

Acrylate resin (UCB)

Pot life >12 months, at room


temperature

Viscosity: 0.72 106 mPa.s at room


temperature

Tg: 170C

Helicopter swash-plate in BMIbased composite

Resin characteristics:

BMI resin

Pot life > 1 day at the injection


temperature (60C)

Viscosity:< 100 mPa.s at T<65C

Tg: 268C

Demonstration boat hull


Resin characteristics:

Thixiotropic acrylate polyester


(UCB)

Pot life >12 months at room


temperature no styrene content

Viscosity: 2000 mPa.s at room


temperature

Tg: 107C

Figure38.121EBcuring:Examplesofpartsandstructures

More recently Boeing designed and built an Electron Beam CureontheFly automated tape
placementmachine.Thistechniqueusesalowenergyelectronbeam,i.e.<500keV.Itisintendedfor
the fabrication of large structures without incurring the large capital and tooling expenditures
inherentinautoclavecuring,Ref.[3846],[3847].Thetechniqueisveryattractiveforproducinglarge
compositesstructuresenvisagedforadvancedaerospacestructures.
InEurope,LabenProelTecnologieDivision,partoftheFinmeccanicaGroup,isinvolvedincomposite
EBcuringusingalayerbylayerlowenergyelectronbeamtechnology,Ref.[3848].

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38.12.2.5 Thermoplastic composites


Thecrosslinkingofcontinuousfibrereinforcedthermoplasticshasalsobeenstudied,Ref.[3828].

38.12.2.6 Facilities
EBprocessingfacilitiesarelargeandexpensive.IndustrialEBunitsareusedforprocessesinvolving
crosslinking of electrical insulation cables, thermoplastic products, rubbers, coatings and adhesives.
Theyarerarelyappliedforthecuringofcomposites.
Organisationswithfacilitiesknowntobecapableofcompositecuringare:

EADSSpaceTransportation,StMdardenJalles,France.

LABENProelTechnologieS.p.A,Firenze,Italy.

AcsionIndustry,Canada.

BoeingwithNASALaRC,USA

38.12.3 Microwave
38.12.3.1 General
Theuseofmicrowavesforcuringboththermosettingcompositesandadhesiveshasbeenstudied,Ref.
[3825], [3830], [3833]. The curing process relies on the generation of temperatures equivalent to
conventional thermal processing. However, the heating effect is localised within the composite and
avoidsthethermalinertiaandheatingofthesurroundingequipment.

38.12.3.2 Composites
In terms of energy consumption, the temperature of the composite can be raised quickly and
efficiently. The consolidation of prepregs relies on pressure applied using vacuum bagging and
autoclaving,[See:38.4].
Curing occurs in a tuneable microwave cavity or a resonant microwave chamber; typically at 2.45
GHz.Theconclusionsmadeinearlyworkwerethat:

Theprocesshadtobeoptimisedtoavoidareasof:

undercuring,or

thermaldegradation(overheating).

Rapidgellingresultedinunacceptablelevelsofporosity.

Combiningthermalheatingandmicrowaveheatingreducedsomeoftheporosityproblems.

Conventional offtheshelf prepregs were not ideally suited to microwave processing, due to
theirresinviscosityandgellingcharacteristics.

Theattractionofthetechniqueisthatthecureprocessingtimeisreduced.Itdoeshoweversufferfrom
thepossibleneedfor:

Specialisedprepregsandadhesives.

Consumables materials and moulds should avoid interfering with the microwave coupling
process.

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38.12.3.3 Adhesives
Results of the microwave curing of conventional AF1632K, EA9689 and EA9391 adhesives showed
that,Ref.[3825]:

Lapshearstrengthswerebetween52%and90%ofthoseachievedbyconventionalthermalcure
cycles.

Thelowervalueswereattributedtothepresenceofvoidagefromtrappedvolatiles.

Totalprocesstimeswerereducedbytwothirdscomparedwithconventionalthermalcuring.

38.12.4 UV curing
TheUVcuringprocessreliesontheuncuredresinbeinginanexposedpositiononthesurfacebeing
irradiated. It has been demonstrated for wet layup configurations containing polyester resins
receptivetoUV.
ThereisnopublishedworkdescribingtheapplicationofUVcuringtohighperformancethermosets,
suchasepoxies,sotheprocessappearstobeoflimitedinterestforspacestructures.

38.13

Preform technology

38.13.1 General
Apreformisanassemblyoffibresinthedesirednetshapeofafinalmoulding,whichcanbeusedin
boththemanufactureof:

polymerbasedcomposites,[See:6.31],and

nonpolymerbasedcompositematerials,[See:Chapter88].

Thedevelopmentofvariouspreformtechnologieshasbeendrivenbyfactorssuchas:

Awishtoreduceoreliminatemanuallabourcostsinassemblingalayupofmaterialpriorto
moulding.

Aneedtointroduce3Dreinforcementtoavoidtheinterlaminar,throughthicknessweaknesses
ofconventionallaminatedplies.

Theuseofautomatedequipmenttocreatecomplexshapesandchangesinsectionnotfeasible
byusingplystacks.

Theuseofperformsisthereforeconsiderednecessaryinsomeapplications,becauseofinadequaciesin
conventionallaminateconstructions,Ref.[3835].
Developments in RTM, resin transfer moulding, [See: 38.7], are providing the greatest incentive to
develop efficient means of preparing fibre preforms. This is primarilyaimed at reducing processing
costs.

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38.13.2 Braids
Braidsareparticularlysuitableforproducingtubularsections,[See:6.31].Theirusein4mstrutshas
beenproposedforlargetrussstructures,Ref.[3811].
The manufacture of tubes by RTM is claimed to improve tolerance to both low and hypervelocity
impactdamageandalsoresistancetomicrocracking,comparedwithUDprepregorfilamentwound
constructions.

38.13.3 Commingled fibre performs


Commingledyarnscontainamixtureofcontinuousthermoplasticfibresandreinforcingfibres,[See:
6.18].
The technique was developed as a means of combining the matrix and reinforcement in a dry
preform.Thepreformisthenheatedtomeltthethermoplastic,andconsolidatedusingpressure.The
useofPEEKthermoplasticfibreshasbeenstudied,Ref.[3836].
Someexamplesofthepossibleapplicationsinclude:

Aircraftstructures,examplesofitemsevaluatedare,Ref.[3836]:

Yspars:AS4(6K)/PEEK150g.

Commingledangleinterlock0/90wovenpreformswithstitched45plies;asshownin
Figure38.13.1,Ref.[3836].

Autoclaveconsolidated,withgraphitetooling.

50%higherstraincapacitythan2Dlaminates.

CommingledAS4/PPS0/90Ibeams.

Potentialspaceapplications,Ref.[3837]:

commingledthermoplasticfibresandUHMcarbonfibres.

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Figure38.131Preformtechnology:Architectureofwovencommingled
AS4/PEEK150g0/90

38.14

Fibre placement

38.14.1 Introduction
FP Fibre placement is an advanced computerautomated production technology for creating CFRP
carbonfibre aerospace structures. The computercontrolled system places carbonfibre layers onto a
mandrel using a direct interface to a CADCAM design system, such as CATIA. This enables direct
informationtransferfromthedrawingtothepart.
Thesystemhastwomainelements:

Head, which has sixdegreeoffreedom feed and roller system to lay CFRP bands onto the
mandrel.Itiscapableofproducingaverywidevarietyofcomplexcurvatureshapes.

Mandrel,whichprovidesasurfaceonwhichtobuildupthefinalshapedpart.

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Thesystem,shownschematicallyinFigure38.14.1,isveryadaptableandimposesfewrestrictionson
thecomponentsthatcanbemade.Inparticular,partsdonotneedanysymmetryofrevolution.
The FP system installed at EADSCASA Espacio can handle thirtytwo 3 mm wide CFRP tows
simultaneously, combining them through a collimator and onto the mandrel. The head can place a
CFRPbandupto100mmwidthatthesametime.

Figure38.141Fibreplacement:Schematicviewofthesystem

Itispossibletostopandrestartplacementofanyoftheindividualtowsandsochangethetotalwidth
of the applied band. This provides a great deal of flexibility in a continuous layup operation, e.g.
whenimplementingholesoraddinglocalreinforcements.
The collimated band is applied to the mandrel by means of a compaction roller. The compaction
pressureiscontrolledautomaticallytoenableplacementofevenlayersoverlighthoneycombcores.

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Thefibrestockmaterialiskeptinacontrolledenvironmentat18Ctopreventtheresinfromstarting
to cure before layup. As the band is placed on the mandrel, the fibres are heated to achieve the
necessary resin viscosity for compaction by the rollers. Figure 38.14.2 shows the main arm and
placementhead,Figure38.14.3showsageneralviewoftheworkingarea.

Figure38.142Fibreplacement:Head

Figure38.143Fibreplacement:Generalviewofworkingarea

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38.14.2 Advantages
38.14.2.1 Productivity
Increasesinproductivityresultfrom:

Reductioninscrapmaterialfrom30%to50%inconventionalprocessingcomparedwith2%to
7%withfibreplacement.

Increasedlayupspeed.

Reductioninthenumberofprecuringoperations,e.g.intermediatedebulking,manualcutting,
positioningoflayers.

38.14.2.2 Complex-shaped components


The fibre placement head can follow almost any complex curvatures with pressure from the
compactionrolleralwaysremainingnormaltothemandrelsurface,asshowninFigure38.14.4.This
enablesaverywidevarietyofcomplex3Dshapes,withmixturesofconcaveandconvexsurfacestobe
formed. Consequently many components, not feasible with filament winding technology, can be
produced.
FP technology can, for instance, produce smooth conetocylinder transitions in a single layup
withoutadditionalmetallicrings.

Figure38.144Fibreplacement:Complexcurvature
38.14.2.3 Single shot lay-up of large structures
Ifmanuallayupisusedforlargestructures,thetimetakenformaterialplacementcanresultinpartial
curing before completion and hence reduction in properties. The higher speed of FP technology
avoidsthisproblem.

38.14.2.4 Holes and reinforcements in components


Mostcompositeaerospacestructuresincludelocalreinforcements,holesandotherdiscontinuities.In
manycases,themanufacturingoperationsneededtoproducetheseareverytimeconsumingandcan
needspecialtools.
In a single production operation, fibre placement can implement hole and reinforcement patterns
simultaneouslywithinthegenerallayup.Thiscanprovidesignificantreductionsintimeandcost.

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38.14.2.5 Fibre placement along specific orientations


In the case of satellitelauncher primary structures, ply orientation is a very important design
parameter in order to achieve optimum performance with minimum mass. Production technologies
suchasfilamentwindingdonotalwaysenableoptimumfibreorientationbecauseacontinuousfibre
trajectory is needed. Fibre placement has none of these restrictions, fibres can be placed at any
orientation(including0and90inconesorcylinders)tomaximiseperformancetomassratio.

Fibreplacementenablestheincorporationofpurelyaxialplies

Figure38.145Fibreplacement:Specificorientations

38.14.3 Repeatability in lay-up and properties


38.14.3.1 General
Based on some preliminary estimations, FP technology gives a plypositioning accuracy four times
better than manual placement, and six times better for angular orientation. Improved layup
tolerancesprovidereducedmanufacturingdeviationsthatleadtoahigherqualityfinalproduct.

38.14.3.2 Complex trajectory placement


Whenlayingupstructuressuchasconesitisnotpossibletohaveaconstantplyangleunlessthefibre
followsacomplextrajectory,asshowninFigure38.14.5.Adeviationfromthiscurvecanleadtonon
optimumthermomechanicalproperties.
Fibre placement can follow any kind of complex path to get the necessary material configuration in
thefinalpart.

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Figure38.146Fibreplacement:Complextrajectories
38.14.3.3 Variable width of band
Variationsinlaminatethicknesscanoccurwheretheoveralldimensionsofacomponentvaryalong
its main axis. For example, in the case of a simple conical shape, if the width of the applied band
remainsconstantitproducesanincreasingfinallaminatethicknessalongthecone(duetoincreased
overlappingatthesmallerendofthecone).
Topreventthiseffect,theFPsystemcanalterthewidthoftheappliedband,hencekeepingtheoverall
thicknessconstantalongthecomponent.Thisisachievedbyincreasinganddecreasingthenumberof
individualtowsmakinguptheband,asshowninFigure38.14.7.

Figure38.147Fibreplacement:Variationofbandwidth

38.14.4 Mixed materials in the same lay-up


Differentmaterialscanbeusedsimultaneouslyinthesamelayupbandbyvaryingthetowsentering
the collimator. For example, in space applications, it is sometimes desirable to reinforce an area by
substitutingahighstrengthfibreforthehighmodulusoneusedinthegenerallayup.Thisenables
thereinforcedareatowithstandhigherloadswithlessmass.
Fibreplacementmakesitpossibletointroduceconductivefibresorotherkindofmaterialforspecific
designneeds.

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Figure38.148Fibreplacement:Mixedmateriallayup

38.14.5 Major advantages of fibre placement compared with other


technologies
38.14.5.1 Filament winding

Lowercost:

higherlayupspeed(filamentbyfilamentcomparedwithbandbyband).

less manufacturing operations (holes and reinforcements made as part of the layup
process)

Betterperformance:

optimumfibreorientation(0and90).

complexshapes(conetocylindertransitionwithoutrings).

optimumreinforcementlayers(materialsandorientations).

Betterquality:

moreaccuratetolerances.

lessmaufacturingdeviations.

Flexibledesign:

noshapelimitations.

nosymmetryofrevolutionrequired.

38.14.5.2 Manual placement

Lowercost:

higherlayupspeed(manualvs.automatic).

less manufacturing operations (holes and reinforcements made as part of the layup
process).

directdatatransferfromdrawingtopart.

lessscrapmaterial.

nointermediatecompaction.

Betterperformance,improvedtolerances(positionandorientation).

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Betterquality:

moreaccuratetolerances(lessmaufacturingdeviations).

betterrepeatability.

Flexibledesign:

largestructurespossibleinasingleprocess.

noshapelimitations.

38.14.6 Examples of European launcher and satellite structures


made by fibre placement
38.14.6.1 Sandwich structures

Ariane5ISS

Cylinder:5.5mdiameter,2.9mheight.

Core:aluminiumalloyhoneycombwithseveralcoredensities.

Skins:differentthicknessesandtransitionsfromsandwichtomonolithic.

Ariane5Adapter1194FP

Cone:2.6mto1.2mdiameter,0.9mheight.

Core:aluminiumalloyhoneycombwithseveralcoredensities

Skins:differentthicknesses.

Ariane5VEBATVOutercylinder

Cylinder:5.5mdiameter,1.2mheight.

Core:aluminiumalloyhoneycombwithseveralcoredensities.

Skins:differentthicknesses.

Ariane5VEBATVInnercone

Cone:5.4mto3.9mdiameter,0.8mheight.

Core:aluminiumalloyhoneycombwithseveralcoredensities.

Skins:differentthicknesses.

38.14.6.2 Monolithic

Ariane5Adapter1194H

Cone:2.6mto1.2mdiameter,0.9mheight.

Skins:differentskinthicknesses,withintegratedCFRPinterfacelowerring.

Ariane5Cone3936

Cone:3.9mto2.6mdiameter,0.8mheight.

Skins:differentthicknesses,withintegratedCFRPinterfaceupperandlowerrings.

Eurostar3000LXCentralTube,Ref.[38-39].

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Coneandcylinderinonecompositepart:1.2mto0.8mconediameter,0.6mconeheight,
0.8mcylinderdiameter,2.1mcylinderheight,2.7mtotalheight,

Skins:differentthicknesses.

38.15

Out of autoclave

38.15.1 Introduction
ThetermOOAoutofautoclaveisusedtodescribeanumberofcompositemanufacturingprocesses
that do not need an autoclave to achieve proper consolidation and cure. These processes can be
broadlygroupedas:

ovencuringofvacuumbaggedprepreglayups.

liquid resin infiltration of fibre preforms, such as RTM, [See: 38.7]; vacuumassisted, e.g.
VARTM;otherderivativeproprietaryprocesses,e.g.SQRTMinfiltrationofprepreglayup,Ref.
[3849].

resinfilminfusion(RFI),aGKNAerospaceprocess,whichinvolveslayingupofdrymultiaxial
fabricinterleavedwithresinfilmthatisthencuredinanovenoronheatedtools,Ref.[3850].

nonthermal cure processes, e.g. EB electron beam, Ref. [3851], microwave, UV cure, [See:
38.12].

otherproprietaryprocesses,e.g.Quickstepmouldingtechnology,whichusesafluidasaheat
transfermediaratherthanagas,[3852],[3853].

As thesize of composite components increase,so does theinvestment necessary for anautoclave of


the appropriate size and its associated facilities. The advantages claimed for OOA processing
comparedwithautoclaving,include:

reducedprocessingtimes.

reducedprocessingcosts.

Savings can result because resins have lower cure temperatures. Reduced tooling costs are also
possiblebecauseofthelowerpressurescomparedwithautoclaving.
ForRTMtypeprocesses,matchedmouldtoolsarenecessary.Somederivativeprocessesforlargethin
partsusetoolingthatincorporatestheresininjectionandventingsystem.Inthesecasestoolingcosts
aresignificantandusuallyneedtobeamortisedoveraseriesofidenticalparts.

38.15.2 Aerospace structural parts


A number of aerospace projects have identified the possible need for OOA composite manufacture,
e.g.EuropeanTANGOproject(Technologyapplicationtotheneartermbusinessgoalsandobjectives
of the aerospace industry) considering composites for large commercial aircraft structure; European
FAST 20XX project (Future HighAltitude HighSpeed Transport, comprising a suborbital and a
hypersonic pointtopoint transport system); NASAs Constellation programme; US Ares V launch
vehicle,civilianaircraftfairings,Ref.[3849].

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However, there are some concerns regarding OOA compared with traditional autoclaved parts,
including:

Overall quality of OOA parts, e.g. higher void content, lower fibre volume fractions, reduced
mechanical properties, because of the lower consolidation pressures. Some OOA processes
claim fibre volume fractions only about 2% lower than autoclaved parts, with void contents
stated from nearzero to <1%. However, the precise values are both process and component
shapedependent.

Geometryofparts:Componentswithdeepdraught,abruptchangesinsectionorsharpcorners
cansufferlocalporosityfrompoorconsolidationandpoorsurfacefinish.Thisusuallyapplies
toprepreglayupsratherthanRTMtypeprocesses.

QualificationismorecomplicatedforRTMtypeprocessesthatcanbeadaptedforaparticular
component. As a result, the final component properties vary with the process parameters.
Considerableeffortisbeingplacedongeneratingdatabasesofmaterialproperties,Ref.[3858].

RTMprocessing of large, thin parts (such as aerodynamic surfaces) need additional vents to
ensureescapeofvolatilesandair.

38.15.3 Composite materials


38.15.3.1 Prepregs
In general, the rheological characteristics of resins in prepregs are modified to enable proper
consolidationunderOOAconditions,i.e.lowertemperature,lowerpressure.
ExamplesofcommerciallyavailableepoxyresinsforprepregsdestinedforOOAinclude:

MTM451andMTM46ACG Advanced Composites Group

CYCOM5320Cytec Engineered Materials

HexPlyM34,EF01,M9.1F/M9.6F,M10Hexcel.

38.15.3.2 Resins
Thetemperatureviscositycharacteristicsoftheresinareimportanttoensureflowandimpregnation
ofthepreformundertheinjectionpressure(oftenfrom0.7MPato1.4MPa).
Epoxies, bismaleimidesand cyanate ester resins are commerciallyavailablefor RTMtype processes.
They are often onepart systems that become less viscous when heated, e.g. HexFlow from Hexcel,
MVRfromACG,CYCOMRTMrangefromCytec.

38.15.4 Tooling
38.15.4.1 Types
AvarietyoftoolingsolutionsarebeingproposedforOOA,including:

ACTsadvancedcompositetools,usuallycarbonfibrebasedcomposites,Ref.[3857].

carbonfoams,Ref.[3854],[3857].

ceramics,Ref.[3855]

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The characteristics for OOA tooling are effectively the same as for autoclave tools, i.e. lowno CTE,
low mass, ease of machining, ease ofincorporatingsystems (heating, venting),resistance tothermal
cyclingoverprocessingtemperatures,longlife.
Carbon foams tools can be used in ovens, Ref. [3857], or made to be selfheating by passing an
electriccurrentthroughthetoolbody,therebyheatingonlythetoolandpartthusavoidingtheneed
foranoven,Ref.[3854].
Heated ceramic tooling, developed under ESAfunding by ire Composites, successfully
demonstratedmouldingflatcarbonfibre/PEEKthermoplasticlaminates,Ref.[3855].
ThetoolcomprisedaPyromeralceramic,Ref.[3856],reinforcedwithcarbonfibrestoprovidethermal
degradationresistance,strengthandlowthermalexpansion.
The properties of laminates made using the Pyromeral tool were determined by mechanical testing
(tensile, compression, inplane shear); bolt bearing; NDT (Cscan), fractography and void analysis,
outgassing, degree of crystallinity (by DSC) and compared favourably with those produced by
autoclave,Ref.[3855].

38.16

References

38.16.1 General
[381]

M.M.Schwartz
Compositematerialshandbook
McGrawHill,1984,ISBN0070557438

[382]

G.Lubin
Handbookofcomposites
VanNostrandReinhold,1982,ISBN0442248970

[383]

M.J.Robinsonetal
Advancedcompositestructuresforlaunchvehicles
SAMPEQuarterly,January1991,p2637

[384]

G.M.Teare
Filamentwindingofsatellitestructures
InternationalSymposium:SpaceApplicationsofAdvancedStructural
Materials,ESTEC
2123March1990,ESASP303,p257260

[385]

C.A.L.Kemperetal
Designandmanufacturingoffilamentwoundthrustcylinder
InternationalSymposium:AdvancedMaterialsforLightweight
Structures,ESTEC,2527March1992
ESASP336,p5156

[386]

K.Lhteenkorvaetal
Tapewindingofthermoplasticcomposites

211

ECSSEHB3220Part4A
20March2011
InternationalSymposium:AdvancedMaterialsforLightweight
Structures,ESTEC,2527March1992
ESASP336,p203206
[387]

M.Wadsworth
Resintransfermoldingofcompositeaircraftstructures
SAETechnicalPaper891042,April1989

[388]

I.Marchbank
AutomatedR.T.M.foranairframecomponent
MaterialsandProcessingMoveintothe90s
EditedbyS.Bensonetal.EuropeanSAMPEConference1989
ElsevierSciencePublishers.p7586

[389]

A.Jiminezetal
DesignandmanufacturingofCFRPringsbyRTM
InternationalSymposium:AdvancedMaterialsforLightweight
Structures,ESTEC,2527March1992
ESASP336,p143148

[3810]

G.C.Sharpless
Advancementofbraiding/resintransfermoldingfromcommercialto
aerospaceapplications
SMETechnicalPaperEM91217,1991

[3811]

A.K.Munjaletal
Designandfabricationofhighqualitygraphite/epoxybraidedcomposite
tubesforspacestructures
35thInternationalSAMPESymposium
April251990,p19541967

[3812]

C.W.Dietrich&D.C.Giedt
Resintransfermoldingandcompressionmoldingprocessingofnozzle
componentsasalowcostalternativetotapewrapping
AIAAPaper932011

[3813]

E.B.Starketal
Anewhighperformanceresinsystemforresintransfermoldingof
aerospacestructures
37thInternationalSAMPESymposium
March9121992,p14211431

[3814]

A.Falconeetal
Resintransfermoldingoftextilecomposites
BoeingDefenceandSpaceGroup,NASACR191505
July1993,139pages

[3815]

A.Wangetal
AnewhightemperatureepoxysystemforRTMapplication
37thInternationalSAMPESymposium
March9121992,p482492

212

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[3816]

K.A.Barrettetal
Injectablebismaleimidesystems
35thInternationalSAMPESymposium
April251990,p10071020

[3817]

E.B.Starketal
Resintransfermolding(RTM)ofhighperformanceresins
35thInternationalSAMPESymposium,April25,1990,p782795

[3818]

J.E.Stockton
Structuralresintransfermoldingofhightemperaturecomposites
34thInternationalSAMPESymposium
May811,1989,p10321040

[3819]

M.CY.Niu
Compositeairframestructures
PublishedbyCommlitPressLtd,January1992
ISBN9627128066

[3820]

G.J.Sundsrud
Advantagesofaonepartresinsystemforprocessingaerospacepartsby
resintransfermoulding(RTM)
Proceedingsofthe14thInternationalEuropeanChapterConferenceof
SAMPE:BroadeningHorizonswithAdvancedMaterials&Processes,
Birmingham,October1993,p.251258,ISBN3952047708

[3821]

F.N.Scott&A.Koorevaar
Computeraidedengineeringoftheresintransfermoulding(RTM)
process
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures,ESTEC
March1994,ESAWPP070,p335340

[3822]

V.M.Karbharietal
Effectofmaterial,process,andequipmentvariablesontheperformance
ofresintransfermouldedparts
CompositesManufacturing,Vol.3,No.3,1992,p143152

[3823]

W.Werner&G.Ziegmann
Developmentoftechniquesforpolymericdiaphragmformingof
continuousfibrereinforcedthermoplastics
ProceedingsoftheInternationalSymposiumonAdvancedMaterialsfor
LightweightStructures,ESTEC
March1994,ESAWPP070,p367371

[3824]

G.H.F.Nayler
Vectrainsulativesupportstructureswithinspacecraft
InternationalSymposium:AdvancedMaterialsforLightweight
Structures
ESTEC,2527March1992,ESASP336,p291298

213

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[3825]

G.B.Gaskinetal
Electromagneticcuringofepoxyadhesivesystems
38thInternationalSAMPESymposium,May10131993
p380390

[3826]

C.B.Saundersetal
Electroncuringoffiberreinforcedcomposites;recentdevelopments
38thInternationalSAMPESymposium,May10131993
p16811691

[3827]

D.Beziersetal
Electronbeamcuringofcomposites
ECCM4,1990,p7378

[3828]

A.B.Strong
Crosslinkingofthermoplasticcompositesusingelectronbeamradiation
SAMPEQuarterly,July1991,p4554

[3829]

C.B.Saundersetal
Recentdevelopmentsintheelectronbeamcuringoffiberreinforced
composites
37thInternationalSAMPESymposium,March9121992
p944954

[3830]

F.Y.C.Boey
Techniquesinthemicrowaveprocessingofthermosetcompositeusinga
highpressureautoclave
23rdInternationalSAMPETechnicalConference
October2124,1991,p1524

[3831]

C.B.Saundersetal
Radiationcurablecarbonfiberprepregcomposites
PolymerComposites,December1988,Vol.9,No.6,p389394

[3832]

C.B.Saundersetal
Radiationcurableprepregcomposites
AtomicEnergyofCanadaLimitedReportAECL9560,1988

[3833]

J.Weietal
Microwaveprocessingofcrossplycontinuousgraphitefiber/epoxy
composites
SAMPEJournal,Vol.27,No.1,Jan./Feb.1991,p3339

[3834]

J.P.Fouassier&J.F.Rabek
Radiationcuringinpolymerscienceandtechnology,1993
Vol.I:FundamentalsandMethods,ISBN1851669299
Vol.II:PhotoinitiatingSystems,ISBN1851669337
Vol.III:PolymerizationMechanisms,ISBN1851669345
Vol.IV:PracticalAspectsandApplications,ISBN1851669388
PublishedbyChapman&Hall,London

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[3835]

J.Brandtetal
Theapplicationofthreedimensionalfibrepreformsforaerospace
compositestructures
InternationalSymposium:SpaceApplicationsofAdvancedStructural
Materials,ESTEC,2123March1990,ESASP303p7177

[3836]

J.Suarez&J.Mahon
Consolidationofgraphite/thermoplastictextilepreformsforprimary
aircraftstructure
TheFirstNASAAdvancedCompositesTechnologyConference,Part1,
p293338(N9330439)

[3837]

C.Blair&G.A.Jensen
Processdevelopmentandcharacterisationofultrahighmodulus,
drapablegraphite/thermoplasticcompositesforspaceapplications
37thInternationalSAMPESymposium,March912,1992
p115127

[3838]

J.Pascual&J.Trigo:EADSCASAEspacio(E)
ApplicationofNewTechnologiesforEurostarCentralTube
Paper161:ESASP581:ProceedingsofEuropeanConferenceon
SpacecraftStructures,MaterialsandMechanicalTesting,ESTEC,
Noordwijk(NL)1012May2005

[3839]

J.Pascual&J.Trigo:EADSCASAEspacio(E)
ApplicationofNewTechnologiesforEurostarCentralTube
ESASP581:ProceedingsofEuropeanConferenceonSpacecraft
Structures,MaterialsandMechanicalTesting,ESTEC,Noordwijk(NL)
1012May2005

[3840]

B.Defoortetal.:EADSST(Bordeaux,F)
Electronbeampolymerizationofacrylatecompositions6:Influenceof
processingparametersonthecuringkineticsofanepoxyacrylateblend
Macromol.Chem.Phys.,202,16,pp31493156,(2001)

[3841]

B.Defoortetal:EADSST(Bordeaux,F)
ModellingoftheEBcuringoffibrereinforcedcompositematerialsfor
aerospaceapplications
Presentation23rdMeetingoftheAdhesionSociety,February2000,
MyrtleBeachSC,USA,pp392394

[3842]

B.Defoorteta:.EADSST(Bordeaux,F)
ElectronBeamcuringofacrylateresinsforcomposites:Modelling
reactionkinetics
45thInternationalSAMPESymposium,May2125,2000,LongBeachCA,
USA,pp22232234

[3843]

B.Defoortetal:EADSST(Bordeaux,F)
InvestigationstoimprovethepropertiesofEBcuredcomposites:A
statusreport
47thInternationalSAMPESymposium,May2002

215

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[3844]

B.Defoort&L.T.Drzal:EADSST(Bordeaux,F)
AdhesionbetweenCarbonfibresandCationicmatricesinElectronBeam
CuringProcessedComposites
46thInternationalSAMPESymposium,610May,2001,LongBeachCA,
USA,pp20632075

[3845]

B.Defoort&L.T.Drzal:EADSST(Bordeaux,F)
InfluenceofThermalPostcuringonElectronBeamCuredComposites
46thInternationalSAMPESymposium,610Mai,2001,LongBeachCA,
USA,pp25502562

[3846]

DLGoodmanetal.
AutomatedTapePlacementwithinsituElectronBeamCure
InternationalSAMPESymposiumandExhibition,May2327,1999,Long
Beach,CA

[3847]

J.W.Burgessetal:BoeingCompany/NASALangley(USA)
DevelopmentofaCureontheflyAutomatedTapePlacementMachine
forElectronBeamCurablePrepregs
46thInternationalSAMPESymposiumandExhibition,May610,1999,
LongBeach,CA;SAMPE2001LongBeach,CAMay610,2001

[3848]

F.Guasti:LABENProelTechnologie(I)
PressureVessels:APossibleApplicationoflowEnergyEBeamcuring
44thInternationalSAMPESymposiumandExhibition,May2327,1999,
LongBeach,CA

[3849]

K.Mason
AutoclaveQualityOutsidetheAutoclave?
HighPerformanceComposites(2006)
http://www.compositesworld.com/articles/autoclavequalityoutsidethe
autoclave.aspx

[3850]

GKNAerospaceDevelopsManufacturingProcessesforComplex
CompositeStructures
http://www.azom.com/news.asp?newsID=6054

[3851]

C.A.Byrne:ScienceResearchLabInc,Ma,(USA)
NonAutoclaveMaterialsforLargeCompositeStructures
ReportNo.A897483(November2000)
Abstract:http://www.stormingmedia.us/89/8974/A897483.html

[3852]

M.Kaiseretal:Inst.frFlugzeugbau,Uni.Stuttgart/EurocopterGmbH
(D)
OutOfAutoclaveManufactureofStructuralAerospaceComposite
Materials
http://www.quickstep.com.au/files/document/165_Out_of_Autoclave_Pr
ocessing_via_Quickstep.pdf

[3853]

QuickstepTechnologiesPtyLtd(Australia)
http://www.quickstep.com.au/

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[3854]

TRLTouchstoneResearchLaboratoryLtd(USA)
CarbonFoamSelfheatedToolingforOutofAutoclaveComposites
Manufacturing
ProposalNo.081X4.069473,NASASBIR2008Solicitation
http://sbir.nasa.gov/SBIR/abstracts/08/sbir/phase1/SBIR081X4.06
9473.html?solicitationId=SBIR_08_P1

[3855]

A.Murtagh:ireCompositesTeo(ire)
ApplicationofThermoplasticCompositeOutofAutoclaveVacuum
ProcessingTechnologytoNonSpaceStructures
EC4706020RPTAFinalReport(October2008),
ESTECContractNo.19729/06/NL/PA

[3856]

Pyromeralhttp://www.pyromeral.com/index.htm

[3857]

ACGAdvancedCompositesGroup(UK)
TechnicalReportNewToolingDevelopments,(March2008)
http://www.advancedcomposites.co.uk/
PSG_Electronic_Files/Tooling_PSG_Files/PDFs/Technical%20Report%20
New%20Tooling%20Developments%20A1
%2016th%20March%202009.pdf

[3858]

ACGAdvancedCompositesGroup(UK)
OutofAutoclaveProcessablePrepregsandResinFilms:AnOverviewof
RecentDevelopmentsandSharedDatabases(2006),Abstract
http://www.sae.org/technical/papers/2006013164

38.16.2 ECSS standards


[See:ECSSwebsite]

ECSSQST70
ECSSQ7071

Materials,mechanicalpartsandprocesses
Datafortheselectionofspacematerialsand
processes

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39
Machining techniques
39.1

Introduction

The various techniques used to machine composites are described and the precautions necessary to
preventdamagingthecomponents.
Thetechniquesusedcanvarywiththeparticularcompositematerial.Aramidcompositesoftenneed
differenttoolsfromthoseusedforcarbonandglassreinforcedmaterials.
Special drill bits are available for composites to overcome the problems of using drills designed for
metals,[See:39.9].

[Seealso:ECSSEHB3221formachiningoperationsrelatedtoadhesivebonding;ECSSEHB3222
formachiningpracticesforinsertsinsandwichpanels;ECSSEHB3223formachiningpracticesfor
boltedjoints]

39.2

Basic rules

39.2.1

General

Themachiningofcompositematerialsshouldmeetthebasiccriteriaof:

Nofraying.

Nodelaminationofthecuredcompositeedge.

39.2.2

Equipment

Standardmachiningequipmentwithsmallmodificationsisoftenused.Thecuttingspeedsandfeeds
useddependupon:

thethicknessofthecomposite,

thetypeofcuttingmethod.

Variouscuttingtoolsareusedforthemachiningoperations,including:

countersink,

cutoffwheels,

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routerbits,

bandsawblades,

highspeedsteeldrills,

reamers.

It is particularly important to keep all the tools sharp, in order to provide good quality cuts and to
minimisethepossibilityofdelamination.
Sufficient backup support of the part to be machined is essential to reduce chipping and
delamination,e.g.byusingaluminium.
Insomecasesmachiningofpolymermatrixcompositescancauselocaloverheatinganddestructionof
properties.Inthesesituationscoolingmethodsshouldbeused.

39.3

Routing

39.3.1

Carbon/epoxy composites

Generally,routingwithahighertorquebutlowspeedrouterworksbest.Diamondcutcarbidebitsare
preferable because of higher feed rates at less operator effort than with a six flute configuration. To
extendthetoollifeandtoincreasethecuttingforce,asuitablecoolantisused(noeffectoncutedge
quality).

39.3.2

Aramid/epoxy composites

ThecuttershowninFigure39.3.1,Ref.[391],achievessatisfactoryresults.
Routingwithaconventionalaircrafttoolsteelroutercanbedifficult,whereastheopposedhelixrouter
canbeusedfor:

Cuttinglaminatesintosections.

Cuttingslotsandnotches.

Trimminghoneycombsandwichpanels.

An opposed helix cutter enables laminates up to 6.4 mm thick to be trimmed without problems. A
conventionalrouterneedsmuchmoreeffortforcompositematerialthickerthan3.2mm.

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Figure39.31Router:Opposedhelixforaramid/epoxy

39.3.3

Trimming and bevelling

39.3.3.1

Carbon and glass reinforced epoxy

Trimmingandbevellingwithaconventionalrouteragainstaguidecanbeusedsuccessfully.

39.3.3.2

Aramid/epoxy

Thequalityofaramid/epoxytrimmededgescanbeimprovedbyusingarouter,asshowninFigure
39.3.2,Ref.[391].
Trimmededgesofaramid/epoxycanalsobeimprovedbysanding.
With diamond cut carbide type router bits, good cuts can be made up to a composite thickness of
about6.9mm.

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Figure39.32Routerfortrimmingaramid/epoxycomposites

39.4

Sanding

39.4.1

General

Thereareseveralimportantpointstobenotedwhensandingcompositelaminates.Thesepointsrelate
tosandingprocessesfor:

Fit or trim,and

Adhesive bonding.

39.4.2

Fit or trim

Guidelinesforsandingcompositescorrectlyinclude:

Usetoolscorrectly;asshowninFigure 39.4.1,Ref.[391].

Usearightanglesanderof20,000rpmorgreater.

Bulkremoval(dry):Use50mmaluminiumoxidedisks.

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Edgedeburring(water):Use50mm240gritto320grit,siliconcarbide.

Addressedgesatproperangle.

Duringsandingoperations:

Donottrytoremoveanydefectsonsurfacesofpartsbysanding.

Donotoversandbeyondtrimareas.

Donotdeburrholes;countersinkholeswithsanders.

Figure39.41Sandingofcomposites

39.4.3

Bonding

Guidelinesforsandingcompositescorrectlypriortoadhesivebondinginclude:

Layouttheareatobesanded.

Use240grit.

Usetoolsof20,000rpmorgreater.

[See:ECSSEHB3223forfurtherguidanceonthesurfacepreparationforbondedjoints]

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39.4.4

Aramid/epoxy composites

Wet paper is used for sanding of aramid/epoxy laminates to provide cooling and also to prevent
buildupofwastebetweenabrasiveparticles.Thepreferredgritsizesare120and240.

39.5

Sawing

39.5.1

Basic rules

Sawingofcuredlaminatescanbesuccessfullyperformedwith:

Band saws,

Circular saws,or

Sabre saws.

The composite is clamped to eliminate vibration that can cause delamination. Saws need frequent
checkingtomaintainsharpness.

39.5.2

Bandsawing

39.5.2.1

General

Normally a fine, offset, highstrengthsteelstaggertooth blade is used. As a general rule, the saw
bladepitchisselectedbythelaminatethicknesstobecutcorrespondingtotheheightofthreesaw
teeth. This cutting method uses the heel rather than the hook of the cutting tooth blade for cleaner
cuts.Thecuttingbladeisalwayssharpenedbeforecutting.
Surfacespeedintherangeof22.9m/sto33m/sareused;with30.5m/spreferred.Thebestfeedrates
arefrom3mm/sto5mm/s.

39.5.2.2

Aramid/epoxy composites

Bandsawcuttingofaramid/epoxyisusuallyperformedwithafinetoothblade,preferablyusingwater
asacoolant.Thebandsawisruninreverse,sothattheheelofthetoothentersthecompositefirst;as
showninFigure39.5.1,Ref.[391].

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Figure39.51Reversebandsawingaramid/epoxylaminates

39.5.3

Circular sawing

39.5.3.1

General

Diamondbladesarepreferredformostcompositematerials.Cuttingspeedsforcompositesnormally
varybetweenabout10m/sto50m/s.

39.5.3.2

Carbon/epoxy composites

A 6.4 mm carbon/epoxy laminate is best cut with acarbidetipped blade andspeed between 10 m/s
and20m/s.
Figure39.5.2showsthat1.3mm/smaximumfeedrateisidealforallpartsupto2.5mmthick,Ref.[39
1].Thickerpartsarecutatproportionatelylowerfeedrates.

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Figure39.52Circularsawing:Feedrateversusthicknessofcompositematerials
39.5.3.3

Aramid/epoxy composites

Aramid/epoxycanbecutsuccessfullyusingacircularmetalslittingsaw.

39.5.4

Sabre sawing

39.5.4.1

Aramid/epoxy composite

SabresawsnormallyusethebladeshowninFigure39.5.3,Ref.[391],tocutaramid/epoxy,whichcuts
the outermost fibres on both sides of the laminate toward the interior. This type of blade has
alternating sets of five teeth in opposed directions. Blade speeds of 2500 strokes per minute are
advisable.
Bladespeedandfeedratesvarywithmaterialthickness.

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Figure39.53Sabresawing:Alternatingtoothbladeforaramid/epoxy

39.6

Countersinking

39.6.1

General

Carbide,highstrengthsteel,diamondplatecountersinkscanbeuseddependingonthecomposite.

39.6.2

Carbon and glass reinforced epoxy

Carbide countersinks have shown good results with optimum combinations of speed and relief
angles.Conventionalcountersinkingtoolsfrom1750rpmto6000rpmhavebeenusedsuccessfully.

39.6.3

Aramid/epoxy composites

Figure39.6.1showsacountersinkusedforaramid/epoxycomposite,Ref.[391].

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Figure39.61Countersinkforaramid/epoxycomposite

39.7

Counterboring

Carbon, aramid and glass reinforced epoxy composites are normally counterbored using carbide
cuttingtools.
Ingeneral,onlyafewcounterborescanbemadepertool,becausetheentirecuttingedgebearsonthe
workpiecematerialduringtheoperation.
Compared with countersinking of carbon/epoxy, [See also: 39.6], counterboring torque and thrust
forcesaregenerally3timeshigher.

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39.8

Milling

39.8.1

Basic Rules

39.8.1.1

General

Toproduceasurfacecutthatextendspasttheedgeofacompositelaminate,theedgeofthelaminate
ismilledfirsttopreventdelamination,asshowninFigure39.8.1.
Theuseoffluorocarboncoolantisadvisablebecauseofitscoolingefficiency.Thecoolantisappliedas
a spray mist during machining; the distance between the spray applicator and cutter is adjusted so
thatfrostformsonthecutter.

Figure39.81Propermillingtechnique
39.8.1.2

Cutter types

Guidelinesfortheselectionanduseofcuttersare:

Ensurethatcuttersaresharp;dullonescausedelamination.

Alwaysusehighspeedsteelcuttersofthefourflute,positiveraketype.

Usecarbidemillingcuttersofapositiveraketype,withchiploadsof0.10mmto0.15mmper
tooth.

Radiusedendmillslastlongerthansquarecorneredones.

39.8.1.3

Carbon/epoxy composites

Highspeedsteelendmillsorcarbidecutterscanbeusedprovidedthattheyaremultifluted.Four
fluteendmillsareadvisableforefficiencyandtoreducethecuttingforcestoapointwherethereis
lesschanceofdelamination.

39.8.1.4

Aramid/epoxy composites

Conventionalflutedcuttersareusedsatisfactorilyatspeedsof0.4m/sandafeedrateof5mm/s.

39.8.2

Plunge-cut milling

Plungecut milling is not recommended, unless there is sufficient backup support to prevent
delamination.

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39.9

Drilling

39.9.1

Basic problems

39.9.1.1

General

Metal working drill bits were not designed for cutting composites and their use can provoke
significantdamagetoacompositearisingfrom:

Abrasivity: Glass/epoxy and carbon/epoxy are so abrasive that only tungsten carbide tooling
candrillthroughthem.

Heating: For metalworking, the tip heats the metal to provide the plastic flow needed for
efficientcutting.Sincecompositescannottoleratethisheat,thecuttingspeedissloweddownto
ensurethattheheatisaslowaspossible.

Rake: Drill designers had to abandon cutting tips with neutral and negative rakes and wide
chisel points because a drill with a neutral rake scrapes the material and causes it to resist
penetration by the drill tip. The operator exerts pressure to drill the hole, and this pressure
causestheheatbuildup.

Pressure:Neutralrakealsotendstopushthereinforcingfibresoutinfront,needingagreatdeal
of pressure to penetrate the piece. This pressure causes the fibres to bend, resulting in furry,
undersizedholes.

Thepressurealsoproducesexcessiveheat,whichcausesgallingandchipdoggingintheresin.

Feed: The release of pressure as the tool bit breaks through the part causes a sudden and
momentary increase in feed rate. As the tool plunges through the last few fibres, the cutter
shaft,notthecuttingedge,removestheremainingmaterial.Theresultischippingandcracking.

Chipformation:Thebestwaytoanalyseadrillingoperationistoexaminethechips.Theideal
chipformforacompositeisadry,easilymovedchipthatlookslikeconfectionerssugar.

Ifthespeedofthecuttingtoolistoohigh,heatmakestheresinstickyandproducesalumpychip;if
the cutting edge is scraping and not cutting the plastic, the chips are large and flaky. Either type
eventuallyclogsanevacuationsystem.

39.9.1.2

Tool design for composites

Factorsinthedesignoftoolsforcompositesinclude:

Positive rake: The reinforcing fibres are pulled into the workpiece where they are sheared or
broken between the cutting edge and the uncut material. Positive rake on the cutting edge
removes more material per unit of time and per unit of pressure than negative rake, but the
morepositivetherake,themoresensitiveandfragilethecuttingedgebecomes.

Chiseledge:Asmallchiseledgeimprovesthepenetrationrate,whichincreasesthenumberof
machiningoperationsperhour.Theoptimumchiseledgeforcompositesisasclosetoapointas
possible.

Chiphandling:Thechipsareproducedandthenremovedimmediatelyabovetheentranceof
the hole. From this point a properly designed vacuum system can dispose of the chips in
conformancewithsafetyandenvironmentalstandards.

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39.9.2

Drill bits for composites

39.9.2.1

General

Tooling has developed that improves greatly the drilling of glass, carbon and aramidepoxy
compositesandtheirhybrids.Sometoolbitsaremadeoftungstencarbideparticlesoflessthan1m.
Figure39.9.1showsexamplesofdrillbitsforcomposites,Ref.[391],where:

Solidshankdrillsareusedinautomaticdrillingequipment.

Twistdrillsareusedinautomaticdrillingequipment.

Drillguidesystemsaredesignedforusewithanairorelectricdrillingmotor.

(a)Solidshankdrill,(b)Drillguidesystem,(c)Flutedtwistdrill

Figure39.91Drillbitsforcomposites
Fittedwithasocketadapter,drillsizesfrom3mmto25.4mmcanbeusedwiththedrillguidesystem.
The internal compression control spring regulator withdraws the tool after drilling. Its pressure
control compensates at breakthrough, where a sudden increase in feed rate occurs as the tool bit
breaksthroughthelastfewfibres.
Partiallydrilledholesareavoidedbecausetheoperatordepressestheunitcompletelyeachtime;no
changeinpressureisfeltastheholenearscompletion.Thedrillsspeedsarebetween1.5m/sto3m/s;
asrecommended.

39.9.2.2

Aramid/epoxy composites

Guidelinesfordrillbitssuitableforaramidcompositeinclude:

Spadedrillsarebestfordrillingaramid/epoxyleavingverylittlefuzzandfrayingattheedges
ofholes.Likecarbidedrills,thesedrillshaveatendencytoburnunderprolongeduses.

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Conventionaldrillscanalsobeusedifafirmsacrificialbackingisusedontheexitsurface.

Twistandflatendedhighspeedsteeldrillsperformquitewell,especiallywithafirmbackupof
thecompositetoeliminatefuzzinganddelaminationattheexithole.

Backup can be provided by leaving the glass peel ply on both sides of the composite during
drilling.A0.08mmlayeroffibreglassonthesurfacesofthecompositeproducescleanentrance
andexitholes.

Drillspeedsrangefrom25,000rpmto35,000rpm.Thehighspeedsteeldrillresemblesatwist
drillflutedontheend.

39.9.2.3

Glass/epoxy composites

Drillswithtitaniumdiboridecoatingimprovethetoollifeintheorderof9times.

39.9.2.4

Carbon/epoxy composites

Guidelinesfordrillbitssuitableforcarboncompositeinclude:

Tungsten carbide drills, shaped like a standard twist drill, can be used successfully; with a
backingplate.Theycanbeusedfor50to60holesbeforeitneedsresharpening.Standarddrills
needresharpeningafterfor5to6holes,typically.

Various types of coolants have been evaluated to prevent drills from breaking, dulling or
burning.AlubricantcalledBoelubehasperformedwell,butwateristhebest.

Toreducesurfacedelaminationduringdrilling,itisadvisabletohavealayerofwovenglassof
0.08mmonbothsidesofthelaminate.

39.9.2.5

Solid carbide daggar drills

Theperformanceofthistypeofdrillbitcanbesummarisedas:

Quitesuccessful,producingacleanholewithlittleornobreakout.

Drillinghasbeenachievedwithoutusingbackupmaterial.

Sincethedaggardrillmaintainsthetoleranceofthehole,noreamingisnecessary.

Daggerdrillsaresuitableforuseinboth:

handheldunits,asshowninFigure39.9.2.

afixedmachineusingairfeed.

Goodresultsareachievedfor

handfedunitsat900rpm.

airfeedunitsat2100rpmwitha1.3mm/sfeedrate.

Drilling carbon/epoxy and metal simultaneously has produced high quality holes and
countersinks.

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Figure39.92Daggardrillinhandfeedunits

39.10

Orbital drilling

39.10.1 Introduction
Orbitaldrillingisineffectthemillingofcircularholes.Thecuttingtoolrotatesintheusualwaybut,at
thesametime,thetoolaxisismovedaroundacircularpathaboutthedesiredholecentreandthetool
isfedintothematerial,asshowninFigure39.10.1.

Figure39.101Orbitaldrillingprinciple
Different hole sizes can be machined using the same tool by altering the diameter of the orbital
movement.Thefinalholediameterisequivalenttothecuttingtooldiameterplustheorbitaldiameter.

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39.10.2 Advantages
Orbital drilling offers a number of advantages compared with conventional machining techniques,
including:

Tighttoleranceholes.

Burrlessholesinmetals.

Delaminationfreeholesincomposites.

Variousholesizesusingasingletool.

Singleoperation,usingonetoolinonesetup.

Goodsurfacefinish.

39.10.3 Drilling parameters


Inordertoobtaingoodresults,threeparametersshouldbeadjusted,i.e.:

Toolrotationspeed,

Orbitalrotationspeed,

Feedspeed.

The correct setting of each of these parameters is essential to optimise the machining and to avoid
unwantedeffects.Eachsettingisestablishedbytestingtheprocessonrepresentativesamples.

39.10.4 Equipment
Figure39.10.2showsaTwinspinorbitaldrillingheadfromNovatorAB(Sweden)mountedtoajig.In
thiscasetheequipmentisbeingusedforcompositemachiningbySaabEricssonSpace.

Figure39.102Orbitaldrilling:Equipmentmountedonajig
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39.10.5 Application examples


Figure39.10.3illustratessomeofthemachiningoperationspossibleusingorbitaldrilling.

Figure39.103Orbitaldrilling:Applicationexamples

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39.11

References

39.11.1 General
[391]

M.M.Schwartz
Compositematerialshandbook
McGrawHill,1984

39.11.2 ECSS standards


[See:ECSSwebsite].

ECSSEHB3221
ECSSEHB3222
ECSSEHB3223

Adhesivebondinghandbook;
previouslyESAPSS03210
Insertdesignhandbook;previouslyESA
PSS031202.
Threadedfastenershandbook;
previouslyESAPSS03208

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40
Manufacturing costs
40.1

Introduction

The selection of materials and appropriate manufacturing processes has important implications
concerning the costs within projects. Composites are used because they offer a range of benefits, of
which masssaving is the most prominent, Ref. [401], [402], [403]. There are often a number of
designs and configurations that fulfil adequately a particular structural configuration. Some of the
competing designs can involve a choice between lightalloys and composites. A part of all design
selectionapproachesistoestablishanacceptablebalancebetweenthe:

totalcostofmanufacture,and

efficiencyofthestructuretomeetitsfunctionalrole.

Thefactorscontributingtothemanufacturingandfabricationcostsofstructuresaredescribed,[See:
40.2].Theitemsconsideredcontributetothedirectaccumulatedmanufacturingcost,i.e.:

materials,

consumables,

processtimes,

capitalequipment,

labour.

Quantifying and allocating manufacturing costs to individual space composite structures and
componentsisdifficultbecause:

designandprocessdevelopmentcostsareveryhigh,

numbersofunitsproducedisoftenverylow,e.g.nomorethanfiveforsatellites,typically,

structuralverificationandqualificationcostsarehigh.

Consequently,withinaproject,itisnoteasytoestablishthetruemanufacturingcostsforindividual
componentsandassemblies.
There is always a strong incentive to retain proven materials and associated manufacturing
technologiesbecausedevelopmentandverificationactivitiesoftenrepresentalargepartofthecosts.

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40.2

Cost drivers

40.2.1

General

Comparedwithaircraftconstruction,thespaceindustryusesfairlysmalltotalquantitiesofcomposite
materials.Itisadvisabletousematerialswithaclearcommercialfuture,i.e.thoseprocuredbymore
thanoneindustrialsector.Wherespecialist,lowvolumeprepregsareconcerned,e.g.UHMCFRP,the
materialcostisveryhighandthechoicelimited.Thesameappliestoothermaterials,e.g.aluminium
lithiumalloys,metalmatrixandceramicmatrixcomposites.
Theissuesthatcontributesignificantlytotheaccumulatedmanufacturedcostare:

Projectcosts,

Massforcostbudget,

Materialsselection,

Designformanufacturing,

Manufacturing,

Toolingandconsumables,

Processingtimes,

Labourcosts,

Partcount,

Unitnumbers,

Productlifeandsourcing.

40.2.2

Project cost drivers

Bygeneralconsensus,thesefactorsare,Ref.[404]:

Specificationenvelope:

massbudget,and

materialsselection.

Qualificationphilosophy.

Standardisation:conflictsbetweenmassandcost.

Methodology:toreducetimeforindividualtasksorprocesses.

40.2.3

Mass for cost budgets

Achievingthemasstargetsorbudgetsisfundamentaltothesuccessofspacestructures.Ifthemass
budgetistoorestrictive,thenmoreexpensivematerialtechnologiescanbeneeded.

40.2.4

Materials selection

Thisisinfluencedbythekeyfactors:

Existingknowledgebase,and

Massbudget:degreeofdifficulty.

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The selection process reflects the naturally conservative philosophy of obtaining the maximum
capabilityfromanexistingtechnologybeforeapplyinganewone.

40.2.5

Design for manufacturing

Aclassicalerrormadeintheearlyyearsofcompositedevelopmentwastoapplyanexistingmetallic
designtothecompositeequivalent.Thisdidnottakeaccountoftheadvantagesofferedbycomposites
and the means of manufacture. Components were not optimised for mass and were invariably
expensive.

40.2.6

Manufacturing expertise

Theexistingavailabilityofmanufacturingfacilitiesandproductionexpertiseisastrongincentiveto
useexistingmanufacturingprocesses.Itenablescoststobemoreaccuratelypredictedbeforemaking
commitmentstoanewcomponentdesign.
Whereanewmanufacturingrouteisnecessary,itisappropriatetoconsiderthe:

Useofasubcontractorwhoalreadyhasthefacilitiesandskillsforthatmanufacturingroute.

Development costs of using a new process, and whether these can be amortised over future
productionorotherprojects.

40.2.7

Tooling and consumables

Toolingis generallya oneoff, nonrecurring cost.For low production runs, cost of tooling is a very
significantcontributoryfactortounitcosts.
Someprocesses,suchasautoclaving,uselargequantitiesofconsumables,suchas:

Baggingmaterials,

Breatherplies,

Peel Plies,

Releasefilms.

Consumablesarerecurringcostsbecausethematerialscannotbereused.Othermanufacturingroutes,
suchasfilamentwinding,usemuchlessconsumablematerial.

40.2.8

Processing times

Whilst a short processing time is desirable, it is not always essential and largely depends on the
componentorassembly,i.e.:

Largecomplexassemblies:Alongcurescheduleneednotbeasignificantcostfactorifonlya
fewunitsarebeingmade.

Smallercomponents(producedinlargernumbers):Reductionofprocesstimesisamajorcost
driver.

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40.2.9

Labour costs

40.2.9.1

General

This remains one of the most difficult items to quantify, because organisations calculating it on a
differentbasis.

40.2.9.2

Direct costs

Thedirectcostsassociatedwiththeactualmanufactureofcomponents,include:

Materialandtoolpreparation,

Lay-Up,

Equipmentoperation,

Demoulding,

Machiningandtrimming,and

Inspection.

Thecostofdesignandtestingisaddedtothesetogiveanoverallfigure.

40.2.10 Part count


40.2.10.1 General
It is important that composite designs offer a reduction in the part count compared with metallic
solutions.

40.2.10.2 Light-alloy
Complexconstructionsinlightalloysareoftenmadeupoftensofindividualcomponents.Theseare
thenfastenedorbondedtogether.Thematerialcostcanbelowbutthefabricationcostshigh.

40.2.10.3 Composites
The aim is to produce a small number of composite components for subsequent assembly. In some
cases, a single part can be feasible, e.g. by cocuring. Whilst the material and consumable costs can
thereforebehigh,subsequentfabricationcostscanbereduced.

40.2.11 Unit numbers


As more components of the same design are made, their unit cost is lower. This is because non
recurringcostscanbeamortisedoveragreaternumbersofunits.Themaincostsare:

design,and

tooling.

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Additionalsavingscanbemadewithin:

Inspectionandtesting.

Improvedconsistentquality.

Somemanufacturingroutesoffergreatercostsavingsthanothers.

40.2.12 Product life and sourcing


Itisalwaysadvisabletodoublesourcematerials,suchasprepregs.Ifitbecomesnecessarytochange
from the first to second choice, the processing will be amenable to the change without incurring
furthersignificantdevelopmentormodificationcosts.
Materials, such as prepregs and adhesives, tend to have a finite commercial life before being
superseded by an improved product. It is advisable to establish the future availability with the
supplierbeforeselectingthatmaterialforanewcomponentorstructure.

40.3

Cost optimisation

40.3.1

Load-carrying structures

40.3.1.1

Eurostar Bus: Inmarsat 2 derivative

AsummaryofthepointsarisingfromaBAestudyforESTECoftheEurostargenericsatellitebusare
described,whichconsidereditsfirstcommercialderivativetomeettheInmarsat2mission,Ref.[404].
It demonstrates the use of composites within the context of an overall project and the cost
optimisationofacommunicationssatellite.
Thecommonfeatureswhichenableonesatellitetobeassessedagainstanotherare:

Firstcost,

Directoperatingcost,

Operatinglife,and

Operationalcapability.

Whilst first cost savings can be made at the expense of other features, cost optimisation through
improvementsinefficiencycanbeachievedwhichdonotadverselyimpactontheotherkeyfactors.
Thefundamentaltradeoffthroughoutanyoptimisationisthatofmassforcost.

40.3.1.2

Mass- cost impact of material selection

Themaincomponentscontributingtothemassandcostofthesatellitebuswere:

Centralthruststructure,

Payloadandequipmentpanels,

Struts,

Bracketsandcleats.

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Thesegroupswerechosentosimplifythecomparativeanalysisbycombiningelementswithcommon
designdrivers.
Table40.3.1liststherangeofcandidatematerialschosenforanalysis,Ref.[404].

Table40.31Costoptimisation:EurostarBus/Inmarsat2study
Material

Specific
Modulus

CTE

Thermal
Conductivity

Costperkg

Al Alloy
AL-Li Alloy
Titanium
Beryllium
HM CFRP
APC 2
MMCp
MMCf

Low
Low
Low
High
High
Medium
Low/medium
High

High
High
Medium
Medium
Low
Low
Medium
Low

High
Medium
Medium
High
Low
Low
Medium
Low/medium

3-5
15-20
15-20
>800
>125
>125
>150
>5000

Key:Procuredmaterialscostsin1989.

For each candidate material, at least two configurations for each of the components were designed;
representing a minimum mass and a minimum cost philosophy. In some cases a midpoint
configurationwasavailablewheretheexistingEurostarbaselinewasnotconsideredtobeminimum
mass.

Figure40.3.1showstherelationshipbetweenmassandcostforthecentralthruststructure,Ref.[404].
Eachlinehasthreepoints;theseare(fromlefttoright):

Minimummass,

Midpointmass,

Minimumcost.

Formassreduction,curveshavingshallowslopesresultinagreatermassreductionperunitincrease
incost.
For cost reduction, curves with the steepest slopes offer greater cost reductions for unit increase in
mass.

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Figure40.31Mass/costsensitivityforcentralthruststructure

Figure40.3.2showsthenextstepoftheentirestructurewithaccumulatedmasscostprofiles,Ref.[40
4].Thisillustratesthat,overall,therearenosignificantwinnersandlosers.Indeed,thedifferencesare
generallyinsignificantcomparedwiththebasicmaterialcapabilitiesintermsofmassandcost.

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Figure40.32Mass/costsensitivityforcompletestructure

Thematerialselectionphilosophiesconsideredwere,Ref.[404]:

minimummassscenario,or

minimumcostscenario.

AsseeninFigure40.3.2,Ref.[404]:

Minimum mass scenario reflects a typical design policy to use existing materials up to their
minimummasslimitpriortoselectingnewmoreefficientmaterials.

Minimum cost scenario is an approach where the most efficient materials are used with a
minimumcostdesignphilosophy.

Thecurrentdesignphilosophy,ortheMin.massscenariohasprovidedagenerallyoptimisedmass
tocosttradeoffbyshowingthatthecostimpactofmaterialswithahigherstructuralefficiencycannot
besupportedinaminimumcostdesign.

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Figure40.33Masstocostenvelopeformaterialimprovements
40.3.1.3

General guidelines

Thesecanbesummarisedas:

Maximiseavailablemassbudget.

Maximisequalificationbysimilarity.

Maximisestandardisationof:

parts,

materials,

methods,and

sources.

Standardfeaturesoritemsarelikelytobethosewhich:

donotimpactonexternalinterfaces,

haveasmallmassimpact,

applytoatleastonethirdofprogrammes.

Usemethodsthatenableautomationandintegrationofprocessesandtasks.

Useexistingmaterialsuptotheirminimummasscapabilitybeforeselectingmorestructurally
efficientoptions.

Theuseofcommongeometryisessential.

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40.4

Cost advantages of composites

40.4.1

Material costs

Historically,compositeshavebeenconsideredtobeexpensiveincomparisonwithestablishedlight
alloys,suchasaluminium.Thedirectmaterialpurchasecostsperkilogramareverydifferent,insome
cases,byordersofmagnitude.

40.4.2

Manufacturing costs

The material costs are typically in the range of 10 % to 25 % of the total manufacturing cost.
Compositesofferopportunitiestoreducecostsonotheraspectsofmanufacturingandfabrication.
Inordertocontrolthetotalmanufacturedcostofacomponentorassembly,theadvantagesoffered
bycompositesthatneedtobeproperlyexploitedare:

Alowerpartcountcomparedwithmetallicdesigns.

Fewerfastenerscomparedwithmetallicdesigns.

Lowermaterialwastagecomparedwithmachinedmetaldesigns.

Reducedmachiningcostsbynetshapeforming.

Cocuringofparts.

UseofpreformsandbroadgoodsinsteadofUDprepregs.

Thereductionandcontroloflabourcostsduringthefabricationstagesalsoshouldbeaddressed.

40.5

Satellite thrust cylinders

Historically, composite satellite thrust cylinders for European space programmes, [See also: 29.12],
havebeenmadebyavarietyofconstructionmethods,including:

Autoclaved,lightalloyhoneycombsandwich.

RibstiffenedCFRPdesigns.

FilamentwoundCFRP.

Thecylindersaremanufacturedbydifferentcontractorsinsmallnumbersforeachprogramme.There
appears to be no general consensus as to which is the most costeffective route for producing a
commonstructuralconfiguration.Itisassumedthatthedirectcostofmanufacturingeachcylinderisa
small proportion of the total programme cost. The dominant factors are the identity of the prime
contractor and the preferred technology within that organisation. The design selection process is
thereforenotdrivenbyimmediatetechnicaloreconomicconsiderationsbecausethereisnotanopen
choice of method of construction. The effective use of existing inhouse technology dominates the
controlofdevelopmentandverificationcostsforaparticularprogramme.

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40.6

Launcher fairing cylinders

40.6.1

General

AstudybyMDSSCMcDonnellDouglasSpaceSystemsCo.investigatedtheconstructionoptionsfor
averylargelauncherfairing,withforebody(ogive)andintertank(ALS),Ref.[405].
The aim of the design tradeoff study was to establish the total system cost sensitivity to structural
mass,andifheavy,butlowercost,monocoquedesignswerefeasible.
Thekeyfactorsconsideredinthetradeoffwere:

cost,

structuralloads,

minimumgaugeconsiderations,

separationsystems,

acousticandthermalprotection.

damagetoleranceto:

hail,and

lightningstrikes.

Allofthesefactorscontributedtotheoverallmassoftheconstructions.
Thegeneralsystemrequirementswere:

Fairingplusadaptermassallocation:15000kg.

Intertankmassallocation:4500kg.

Cylindergeometry:10.8mdiameter.

Costamortisedover120unitsover10years.

40.6.2

Potential fairing designs

40.6.2.1

General

ThedimensionsandprospectiveconstructionsareshowninFigure40.6.1,Ref.[405].Informationis
presentedforthefairingcylinderandcoversthedirectfindingsonly.

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Informationispresentedforthefairingcylinderandcoversthedirectfindingsonly.

Figure40.61Candidatefairingandintertankconstructions
40.6.2.2

Mass-cost analysis

The mass and cost of respective fairing constructions are shown in Table 40.6.1, Ref. [405]. A
breakdownofthecontributorycostsforthedifferentdesignsisshowninFigure40.6.2,Ref.[405].

Table40.61Launcherfairingconstructions:Massandcostofvariousdesigns
Constructions

UnitMass(kg)

UnitCost($x1000)

GRP Monocoque
CFRP Monocoque
Al-Li Isogrid
GRP Sandwich
CFRP Isogrid
CFRP Sandwich
CFRP Corrugated
CFRP Skin/Stringer

26360
15225
7725
6910
5090
5020
4865
4455

6800
15100
8300
11800
11300

Key:designsfordetailedexamination.

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Comments:
Miscellaneous Support, includes:
design engineering,
planning,
operations support,
QA,
business management,
shipping.

Other, includes common items, e.g.:


utilities,
separation hardware,
access doors,
nose cap.

Figure40.62Fairingcylindercostsfordifferentdesigns(lifecyclecostsperunit)

Basedonlowerproductioncosts(fromcostbreakdowns),theoptionsselectedfordetailedevaluation
were:

CFRPmonocoque,and

CFRPsandwich.

A key to producing lowcost structures is to minimise the part count. This reduces design analysis,
development and tooling costs. Failing to achieve it accounts for the high miscellaneous support
costsseenwiththeisogrid,corrugatedandskin/stringerconcepts.

40.6.2.3

Design-construction trade-off

In addition to cost analysis, a decision analysis process was used to screen options against several
weightedcriteria;showninTable40.6.2,Ref.[405].Thesecriteriadefinethetotalevaluationscores.

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Table40.62Launcherfairings:KepnerTregoetradestudyevaluationcriteria
Criteria

Non-recurring
cost
Recurring cost

Definition

One time DDT and E

Production, launch, flight and operations costs


Total life costs of the option, sum of nonLife cycle cost
recurring and recurring costs
The capability of the option to be
manufactured and assembled with relative
Producibility
ease and simplicity. The relative degree of the
design complexity of the option
Mass
The physical mass of the option
The ease with which the option can be
Maintainability retained in or restored to an operational
condition
The capability to readily inspect the part as
Inspectability processed or following field or transportation
use
The capability to repair a part damaged or
Repairability
found to be discrepant during fabrication and
assembly
The ability to modify the design and
Flexibility
construction for number and size of openings
or alter geometry (i.e. diameter and length)

Weighting
Factor

4
9
10
8
7
4
5
4
4

ThefairingcylindersectionscoresareshowninFigure40.6.3,Ref.[405],wherealowscoreindicatesa
highmassorahighcost.
The criteria weights and scores were reached by consensus between the MDSSC and Hercules
concurrentengineeringteams.
The CFRP monocoque and sandwich constructions achieved the highest scores and underwent
evaluationintheprocesstradeandcostanalysisrefinements.

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Figure40.63Launcherfairingcylinder:KepnerTregoeevaluationscoresforthe
sectiondesigns

40.6.3

Selection of designs

40.6.3.1

Fairing cylinder

The CFRP sandwich was considered the best candidate for the fairing cylinder, with CFRP
monocoqueasthefirstalternative,because:

Thesystemcostsensitivitytomassforthemonocoquewasunknownandpossiblyhigh.

Themassmarginapplied,ifnecessary,addeddurabilitytothelightweightsandwichdesign.

Themonocoquedevelopmentofferedlittlebenefitforimprovementoftheexistingvehicle.

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40.6.3.2

Intertank

Thedatawereevenmoreconclusivelyinfavourofasandwichconstruction.

40.6.3.3

Forebody

Thethermal,lightningstrike,erosionresistancemadethesemimonocoquedesignwithringstiffeners
moreappropriate.

40.6.4

Process and material trade-off

40.6.4.1

General

Variousoptionsforfabricatinglargecompositesectionswerestudied.Automationhadahighpriority
inordertoavoidthehighcostsofhandlayup.Alsoincludedwere:

Ancillarystructures:

stiffeners:longitudinalandcircumferential,

separationrails.

Materials:

fibres,

resins,

adhesives,and

corematerials.

NDTtechniques.

40.6.4.2

Sandwich fairing

TheaccumulatedcostsforthedifferingprocessesappliedtoasandwichfairingareshowninFigure
40.6.4,Ref.[405].Itillustratesthatthechoiceofprocesshasasmalleffectonfinalcost.Thehighest
andlowestcosttotalsdifferbyonly10%.Thisismainlybecausethecompositelayupprocesssimply
generates a large panel and most of the cost of the fairing is incurred later during assembly and
generalsupportactivities.
Anaccurateassessmentofprocessreliability,producibility,riskminimisationandothercriteriafrom
theKepnerTregoeevaluationareimportant;asshowninFigure40.6.5,Ref.[405].
Basedontheprocessingassessmentasawhole,thebestoptionscanbesummarisedas:

Fairingcylinderandintertank:Broadgoodsdispensingandfilamentwinding.

Forebody:Filamentwindingandfibreplacement.

40.6.4.3

Materials selection

Forthesandwichconstructions,anintermediatemodulus,IM,carbonfibreCFRPwithanaluminium
honeycombcorewaspreferred.

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Figure40.64Launcherfairing:Unitlifecyclecostsforsandwichfairingcylinder
designsfordifferentfabricationprocesses

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Figure40.65Launcherfairing:KepnerTregoeevaluationscoresforprocessesto
fabricatethemonocoqueandsandwichcylinder

40.7

Thermoplastic versus thermoset

40.7.1

General

Within the composites industry, claims are made that the manufacturing costs for continuous fibre
reinforced thermoplastic composites components are lower than the equivalent thermoset versions.
The potential savings are associated with the shorter processing times for thermoplastics compared
with thermosets. This invites questions as to why thermosets still dominate aerospace applications,
and why thermoplastic composites are virtually absent from space structures and programmes,
particularlyinEurope.

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ThepositionofEuropeanspacecontractorscanbesummarisedas:

Theproductionrunsforthemajorityofsatelliteconstructionsaresmallanddonotwarrantthe
useofthermoplastics.

The range of commercial thermoplastic materials available, especially with higher modulus
fibres,issmallincomparisonwiththermosetprepregs.

Thermoplasticprepregsaremoreexpensivetopurchasethantheirthermosetequivalents.

There is little or no incentive to invest in thermoplastic forming technology when


comprehensivethermosetmouldingfacilitiesexist.

Opportunitiesareidentifiedwherethermoplasticscanbeappropriate,solelyonthegroundsoflower
total manufactured costs compared with thermosets. Other technical benefits associated with
thermoplasticsarenotconsideredhere.

[Seealso:6.16fortechnicalaspects;6.27foreconomicrelatedfactors]

40.7.2

Recurring spacecraft components

40.7.2.1

General

A cost study by TRW Space and Technology Group, USA, identified some opportunities for
thermoplastics,Ref.[406].Thestudypremisewasacommercialdemandforsmall,lightweight,low
costsatellitesinthefuture,whichneedslargescaleproductionofcomponents(exceeding1000units)
withalowcostperunit.

40.7.2.2

Processes

Processeswerecomparedwithautoclavingofathermosetdesign;thoseevaluatedwere:

Superplasticdiaphragmforming.

Hottransferpressmoulding.

Filamentwinding.

40.7.2.3

Components

Thecommonbaselineconfigurationsstudiedwere:

Cchannel(diagonalbrace):

Dimensions:380mmx25mm.

Mass:36g.

Angletab(topreventbucklinginbeams):

Dimensions:190mmx19mm.

Mass:10g.

Antennamastsupportstruttube:

Dimensions:2.4mlong,57mminternaldiameter,1.27mm.wallthickness

Mass:1150g.

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40.7.2.4

Unit costs

Unitcostsweredeterminedforproductionnumbersof1,10and100units.
Theeconomicbasedassumptionsincluded:

Labourcostsincludedbothdirectandindirectcosts,

An85%learningcurveforfabricationprocesses,

Vendorsuppliedcompositematerialcostsatproductionvolumes,

Developmental startup costs for thermoplastic processes not included in the manufacturing
costperpart,

Labourcostsbasedon:

partcycletime,

learningcurve,and

degreeofskillrequired,

Typicalfabricationoperationsincludedinlabourcosts:

plycutting,

layup,

bagging,

consolidation,

trim,and

inspection.

Costestimatesforcomponentsconsistedof:

nonrecurringtoolingcosts,i.e.design,fabricationandmaterials,

diaphragmformingcageassemblydepreciation,

recurring material costs and recurring fabrication labour costs derived from the cycle
times.

Itemsnotincluded:

autoclavedepreciation,

equipmentpurchasecostsforthethermoplasticprocessing(smallcomparedwiththecost
ofoperatinganautoclave).

The relative costs for the selected components were calculated and showed that cost reductions are
possibleforthermoplasticswhenunitnumbersexceed10;asgiveninTable40.7.1,Ref.[406].

For1unitorfor100units,thecostimplicationsareverydifferentforeachcomponent,asshownin
Figure40.7.1,Ref.[406].Itillustratesthatthermoplasticsarenotattractiveuntilacertainnumberof
unitsaremade,e.g.atleast10forCchannelandangletabs.Whereasfilamentwoundstrutsmadeof
thermoplasticsarefavourableforanynumberofunitscomparedwithautoclaving.Thisisalsotruefor
filamentwoundthermosetwhencomparedwithautoclaving(notincludedinthestudy).

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Table40.71Selectedthermoplasticcomponent:Cost/producibilitytradeoff
analysis

T300/934Epoxy

IM7/PEEKThermoplastic

Fabrication
Method

Total
Fabrication
(hrs/part)(2)

Fabrication
Method

Manufacturing
CostReduction
perPart(1)

TotalFabrication
(hrs/part)(2)

10

100

off

off

32%

49%

0.35

20%

43%

20(3)

40%

43%

Cchannel

Autoclave

16.5

Superplastic
diaphragm
forming
AngleTabs(4)

Autoclave

1.1

Hot transfer
press moulding
AntennaMast

Autoclave

34

Filament
winding

Key:
(1)Includesnonrecurringtoolingandrecurringfabricationcosts.
(2)Actualfabricationtime(doesnotincludetrim/inspectiontime)
(3)Includescomputerprogrammingtimeforwindingpattern
(4)Basedonshipsetsofsixparts

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Figure40.71Thermoplasticcomponents:Manufacturingunitcostsasafunction
ofproductionvolumes

Table40.7.2liststhemajorcostcontributorsforproducinglownumbersofunits,i.e.from1to5,Ref.
[406].Thisshowscoststobedominatedbytooling.
Whenhigherunitnumbersaremade,labourcostspredominate.Thisiswherethermoplasticsofferthe
highestbenefits.

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Table40.72Selectedthermoplasticcomponents:Relativemanufacturingcosts
andmajorcontributorstocost
Methodof
Manufacture

Relative
Costof1
Unit

Relative
Costof100 MajorCostItems
Units

MajorCostItems

100

Tooling:71%
Labour:26%

100

Labour:95%

99

Tooling:71%
Labour:26%

96

Labour:93%

51

Labour:84%

100

Labour:93%

CChannel

Autoclave
thermoset
Autoclave
thermoplasti
c
SDF
thermoplasti
c
Autoclave
thermoset

114
100

Tooling:64%
Equipment:23%
Labour:11%
Labour:70%
Tooling:25%
Angletab

Autoclave
thermoplasti
c
H-TPF
thermoplasti
c
Autoclave
thermoset

98

Labour:69%
Tooling:25%

92

Labour:90%

250

Tooling:85%
Labour:13%

57

Labour:74%
Materials:16%

100

Labour:52%
Tooling:37%
Materials:11%

100

Labour:81%
Materials:16%

102

Labour:75%
Materials:22%

58

Labour:48%
Materials:46%

Strut

Autoclave
thermoplasti
c
FW
thermoplasti
c

110
87

Labour:45%
Tooling:41%
Materials:14%
Labour:41%
Tooling:36%
Materials:23%

Key::largestcontributorfirst

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40.7.3

Thermoplastic composites in aircraft

BothFokker(NL)andDornierLuftfahrt(D)usethermoplasticpartsinproductioncomponents,e.g.:

Fokker50iceprotectionplates:

CetexPEI.

Dornier328iceprotectionplatesandlandingflapribs:

CetexPEI/T300(fromTenCate).

Ref.[407]givesinformationofthecostofthelandingflapribs.
The components are relatively simple shapes, with typical dimensions of 375 mm x 140 mm. The
preferredmanufacturingrouteisbyhotpressing.
Thepossibleconstructionscostedwere:

Aluminium(Al3.1364),

ThermoplasticCetexPEI/T300,

ThermoplasticICIPEEKAPC2/AS4,

UDEpoxyCFRP(6376/HTA7),and

FabricEpoxyCFRP(W3T28242/F593).

Thethermoplasticvariantswerecostedforboth1and3ribspercycleanda20%reductioninmaterial
prices.Figure40.7.2showsabreakdownoftherelativepartcosts,Ref.[407].
Itwasconcludedthatthethermoplasticvariantwascosteffectivecomparedwiththermosets,butnot
withaluminiumunlessthreepartsweremadesimultaneouslyineachcycle.
ThehighmaterialcostofPEEKAPC2isadisadvantagecomparedwiththecheaperCetexPEI.

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Key:

Calculation basis: Landing flap rib thickness: 1.25 mm in CFRP, 1.0 mm in Al.
Area: 0.11 m. Mass: 220g (CFRP), 300g (Al). For 400a/c, all costs in 1991,
numbersincludequalitycostsandmaterialsurcharges.

Figure40.72Relativepartcostsforthermoplasticaircraftcomponents:Dornier
328landingflaprib

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40.7.4

Conclusions

Someconclusionsonthecostviabilityofthermoplasticcompositesinclude:

Autoclave moulded thermoplastic composites do not offer any costsavings over autoclaved
mouldedthermosets.

Smalltomediumsized,simpleshapescanbemadeatlowercostinthermoplasticscompared
withthermoplastics,providingthatrapidformingtechniquesareused.

Unitproductionneedstoexceedacertainnumberbeforeitisattractivetousethermoplastics.

For complex shapes, the cost difference between thermoset and thermoplastics reduces
considerably.

The use of thermoplastic composites in space structures can be considered where unit
productionnumbersarerelativelyhigh,suchasfor:

launchers

commonsatellitestructures,e.g.withinseriesofcommunicationandmicrosatellites.

40.8

Automation

Automated composite processing is only of value if it achieves costsavings, compared with labour
intensiveactivities,whichexceedthecapitalequipmentcost.
Thebasicareaswherethiscanbethecaseare:

Cuttingandstackingofprepregs,i.e.lay-up.

Highnumbersofunitsproduced.

Giventhelimitedconsumptionofmaterialsforsatelliteconstructions,automationcanbedifficultto
justify.Themarketforlaunchersisdifferentbecauseunitnumbersarehigherandalargeramountof
materialishandledandprocessed.
Fordesignersofautomatedsystems,thecosteffectivenessisanimportantdesignparameterfromthe
originaldesignconceptstage.Alargerpercentageofthefinalcostofapartisdeterminedintheearly
phasesofthelifecycleofaproduct,i.e.atthedesignphaseasopposedtoproductionphase.
Astudyontheopportunitiesforautomationconcludedthat,Ref.[408]:

Thecosteffectivenessofamanufacturingprocessisatradeoffbetweenrawmaterialcostsand
downstreammanufacturingcostsdeterminedbythatmaterial.

High cost, valueadded materials are most costeffective since they need the least amount of
labour during processing. i.e. 3D constructions, broadgoods, preforms, braids and fabrics as
opposedtoUDtape.

Automatedtechniqueswhichreducelabourcanuselowcostmaterialseffectively,e.g.:

automatedtapelayup,and

filamentwinding.

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40.9

Cost analysis methods

Severalattemptshavebeenmadetodevisemethodsforquantifyingthecostofproducingcomposite
componentsbydifferentmanufacturingroutes,Ref.[406],[408],[409],[4010],[4011].
Generally, such exercises are only of value where the number of component units produced is
reasonablyhigh.
The analysis methods attempt to compare different processes that often produce subtly different
components. The methods often make assumptions and can only produce valid results if there is
agreementon:

Costingoflabourandoverheadrates.

Equipmentcosts.

Allocationofdevelopmentcosts.

40.10

References

40.10.1 General
[401]

UniversityofDelaware
Compositedesignguide
Issue9,1983

[402]

G.Lubin
Handbookofcomposites
VanNostrandReinhold,1982

[403]

V.M.Karbhari&D.J.Wilkins
Selectingmaterials,processes&shapes:gettingitrightthefirsttime
37thInternationalSAMPESymposium
March912,1992,p13791391

[404]

B.A.Reid&A.Pradier
Costoptimisationofloadcarryingstructures
ProceedingsoftheInternationalSymposiumSpaceApplicationsof
AdvancedStructuralMaterials
ESTEC,TheNetherlands,2123March1990,ESASP303,p397402
BAe TP8598 - Cost optimisation of load carrying structures, Phase 1
Final Report, ESTEC Contract No. 7529/88/NL/PH
BAe TP8673 - Cost optimisation of load carrying structures, Phase 2
Final Report, ESTEC Contract No. 7529/88/NL/PH
BAe TP8683 Cost optimisation of load carrying structures
guidelines, Phase 1 Final Report, ESTEC Contract No.
7529/88/NL/PH

[405]

M.J.Robinsonetal
Advancedcompositestructuresforlaunchvehicles
SAMPEQuarterly,January1991,p2637

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[406]

E.M.Silverman&W.C.Forbes
Costanalysisofthermoplasticcompositesprocessingmethodsfor
spacecraftstructures
SAMPEJournal,Vol.26,No.6,November/December1990,p915

[407]

W.Werner
Costeffectivenessofstructuralapplicationsoffibrereinforced
thermoplastics
ProceedingsoftheInternationalSymposiumAdvancedMaterialsfor
LightweightStructures,ESTEC,TheNetherlands
2527March1992,ESASP336,p185190

[408]

M.F.Foley&E.Bernardon
Thermoplasticcompositemanufacturingcostanalysisforthedesignof
costeffectiveautomatedsystems
SAMPEJournal,Vol.26,No.4,July/August1990

[409]

M.F.Foley
Technoeconomicautomatedcompositemanufacturingtechniques
SAMPEQuarterly,January1991,p6268

[4010]

E.Wang&T.Gutowski
Costcomparisonbetweenthermoplastic&thermosetcomposites
SAMPEJournalVol.26No.6,Nov/Dec1990,p1926

[4011]

T.Gutowskietal
Developmentofatheoreticalcostmodelforadvancedcomposite
fabrication
CompositesManufacturing,Vol.5,No.4,1994,p231239

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41
Repair of composites
41.1

Introduction

Damage to composite structures has been studied, and the types of damage categorised, [See: 41.2].
Repairconceptshavebeendevelopedforlaminatesandsandwichstructures.
Themeansofcategorisingtypesofdamagearedescribed.Thevariousrepairconceptsdevelopedto
restorethepropertiesofthestructurearepresented,[See:41.4].

41.2

Damage classification

41.2.1

Life-histories of composite structures

NASA and prime aircraft contractors have compiled life histories of composite structures. This
showedthatnearlyalltypesofdamagetostructuresoccurfrom:

groundhandlingduringassembly,or

maintenance,and

impactofforeignobject.

[See:41.3forallthetypesofdamagethatneedtoberepaired]

41.2.2

Inspection and criticality of damage

Each of the accidental damage types are assessed using various inspection techniques and then
classified regarding their criticality. The inspection techniques commonly used, either singularly or
combined,are,[Seealso:Chapter34]:

Visualexamination.

Tappingtest.

Ultrasonicexamination.

Xrayexamination.

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41.2.3

Repair zones

41.2.3.1

General

The aircraft industry usually divides a structure into repair zones, and determines the allowable
damageforeachzone,Ref.[413].Thestructuralcomponentscanbeclassifiedas:

Structural components(safelifedesign)

Primarystructuralcomponents(failsafedesign)

Secondary structural components

41.2.3.2

Structural components (safe-life design)

Such parts are classified as those whose failure can result in a significant loss of structural
performance,i.e.launcher,satelliteorspacestructure.
The repair concept should meet all the aspects of a safelife design. If it cannot, the whole part is
scrappedandreplaced.

41.2.3.3

Primary structural components (fail-safe design)

Failure of a primary component can have serious consequences on the operation of a structure, e.g.
reducing the performance of a safelife component under cyclic loading. All such components are
subjecttofurtherinspection.
A repair to a damaged primary structure parts has to guarantee the original strength and stiffness
throughouttheinspectioninterval.

41.2.3.4

Secondary structural components

Failurehasnodirectorimmediateeffectsonthesafeoperationofsecondarystructuralparts.
Repairsarenormallyforcosmeticreasonsandreconstitutethecomponentprofile.

41.3

Damage categories

41.3.1

Impact energy levels

The types of damage which lead to the failures, [See: 41.2], are usually classified by their impact
energylevel,i.e.:

Lowenergyimpactatmoderatespeed,e.g.:

handlingincidents,

droppingatoolduringassemblyormaintenance.

Highenergyimpactathighspeed,e.g.:

hail,

smallstonesfromtherunway.

Highenergyimpactatveryhighspeed,e.g.:

Inorbitdebris,

meteoroids.

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41.3.2

Damage types

41.3.2.1

General

The damage produced by each type of impact is categorised and a suitable repair procedure
considered,[411],[412],[413].

41.3.2.2

Scratches

Thedamagehasnoeffectonthestructuralstrength,butisrepairedinordertopreventasubsequent
attackofthepartbyhumidity,UV,particleradiationoratomicoxygen.

Figure41.31Damagecategories:Scratch
41.3.2.3

Notches

The damage does not extend through the full thickness of the part. The effects on the mechanical
performancedependonthedepthofthenotchrelativetothecomponentthickness.

Figure41.32Damagecategories:Notch

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41.3.2.4

Chipping

Thisisalocalfracturewithseparationofthesurfaceplies.Theeffectonthemechanicalperformance
depends on the thickness of the part. Repair is necessary to prevent the structure from subsequent
attackbyexternalagents,e.g.humidity,radiation,atomicoxygen.

Figure41.33Damagecategories:Chipping
41.3.2.5

Debonding

An example is the separation of sandwich skin and the core. The effects depend on the size of the
separatedarea.Repairofthedamagezoneisnecessaryiftheseparatedareaisgreaterthanaspecified
value.

Figure41.34Damagecategories:Debonding

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41.3.2.6

Delamination and dents

Thisoccursduetotheseparationorfromalackofadherencebetweentwopliesofalaminate.Itisof
major importance, especially in thin compressionloaded panels (stability failure) or in thick panels
subjected to interlaminar shear loading. Delaminations are repaired to retain the mechanical
performance.
The combination of delamination and debonding dents often occurs after an impact on the
structure.Dependingontheenergyleveloftheimpact,thefibresorthepliescanbebroken.

Figure41.35Damagecategories:Delamination
41.3.2.7

Perforation

Dependingontheimpactenergy,aperforationcanaffectpartorallofthecomponentthickness.Ithas
majoreffectsonthecompressionpropertiesofastructuralcomponent.Perforationalsocausesleaksin
tanksorpressurisedstructures.

Figure41.36Damagecategories:Perforation

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41.4

Basic repair concepts

41.4.1

General

Therepairprinciplesoftheaircraftindustry,whicharebasedontheFAAregulations,statethat:
Aftertherepairtoastructuralpartmadeofcompositematerials,thereshouldbenodegradationin
theultimatedesignstrengthofthepartforitsremainingservicelife.

41.4.2

Basic types of repairs

Repairsareusuallymadebyreinforcingthedamagedcomponentwithametalorcompositepatch.
Theprincipalmethodsare:

Flushrepairs,wherepatchesarebondedorcuredinplace,[See:41.5].

Externalrepairs,wherepatchesare:

bonded,[See:41.6].

bolted,[See:41.7].

TypicalrepairconceptsareshownschematicallyinFigure41.4.1,Ref.[411].

41.4.3

Repair selection

Thegeneralapproachwithintheaircraftindustryisthatthechoiceofarepairconceptisdefinedinthe
appropriatestructuralrepairmanuals,anddependsonthe:

typeofdamage,[See:41.3].

criticalityofthedamagerelatedtotheimportanceofthestructuralcomponent,[See:41.2].

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Figure41.41Basicrepairconcepts

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41.5

Flush repair concepts

41.5.1

Applications

Flushbonded patches of composites can be necessary to rebuild the originally smooth surface of a
damagedstructuralcomponent.

41.5.2

Post-repair properties

Testresults,Ref.[414],showthatflushrepairsprovidethemosteffectiverestorationoftheoriginal
strength,i.e.withoutdefect.
Thestrengthrecoveryisabout60%forthicklaminates,whichishigherthanthetypicallystated40%
to60%ofultimatestrength(designultimatestrength).

41.5.3

Design

Thepossibledesignsofaflushrepairare,Ref.[415]:

Theremovedmaterialisreplacedinthesameorientationandthesamestackingorderthatused
intheoriginalcomponent;asshowninFigure 41.5.1.

Theremovedmaterialisreplacedparalleltothesurface;asshowninFigure41.5.2.

TheparallelmethodisusedbyAirbusIndustrieandprovidesthemaximumbondstrengthbetween
thecomponentandthepatch.Thisconceptisalsocheaperthantheothermethodtoimplement.

41.5.4

Manufacture

Both types of repairs are cured in place using heatblankets and special types of vacuum bags.
Additional cover plies and the use of an adhesive film between the component and the patch are
advised;asshowninFigure41.5.3.
Ifthecomponenthasalreadybeeninservice,thelaminateisdriedinordertorecoverythemaximum
strength.

Figure41.51Typicalflushrepair

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Figure41.52Flushrepair,usedbyAirbusIndustrie

Figure41.53Flushrepairwithadhesivefilmandcoverplies

41.6

Bonded external repair concepts

41.6.1

Applications

An external patch offers an intermediate level of complexity and cost. It is usually used for lightly
loaded,thinlaminates.

41.6.2

Post-repair properties

The strength recovery is typically between 25 % and 60% of the original strength, Ref. [414]. This
indicates that the design strength (typically 40 to 60% of the ultimate strength without defects) is
possible.
The curing process is a significant parameter regarding strength recovery; the higher the curing
temperature,thehigherthestrengthofarepairedcomponent.

41.6.3

Design

Thedesignvariesdependingonwhetherthepliesareprecuredorcuredinplace,[See:Manufacture].

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41.6.4

Manufacture

Patchesareeither:

Precured;asshowninFigure41.6.1,or

Curedinplace;asshowninFigure41.6.2.

Ifthecomponenthasalreadybeeninservice,therepairareaisdriedbeforethepatchesarebondedin
ordertomaximisestrengthrecovery.

Figure41.61Externalrepair:Precuredpatches

Figure41.62Externalrepair:Curedinplace

41.7

Bolted external repair concepts

41.7.1

Applications

Boltedrepairsarenormallyusedfor:

Delaminationinsignificantcomponents,e.g.skin/stringerstructures,

Preventionofpeelingwithinabondedexternalpatch.

Lightlyloaded,structuralcomponentsorsecondarypartscanberepairedbythismethod.

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41.7.2

Post-repair properties

For structural parts, the repair has to restore at least the ultimate design strength; typically 40 % to
60%oftheundisturbedultimatestrength.

41.7.3

Design

Thedesignvariesdependingonthe:

Location

Useofametalpatch,or

Useofaprecuredcompositepatch;asshowninFigure41.7.1.

Special care is taken when drilling the holes for fasteners to prevent additional delamination of the
laminate.
A sealant is used between the CFRP component and the metal patches to inhibit galvanic corrosion
problems.
Oftenblindfastenersareusedbecausetheaccesstobothsidesofastructuralcomponentisreduced.
Blindfastenershavelowpulloutstrength;thistypeofrepairisnormallyusedfortemporaryrepairs
only.

41.7.4

Manufacture

Repairstoadamagedcomponentaremadebyusingmetalorcompositepatcheswhicharesecured
by:

Boltingonly.

Bondingandbolting.

[Seealso:Design]

Figure41.71Boltedandbondedrepairusingacompositepatch

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41.8

Sandwich structure repair concepts

41.8.1

No core damage

Whenthehoneycomborfoamcoreofasandwichstructureisintact,therepairschemeisthesameas
forathinlaminatedcomponentaccessiblefromonlyoneside,[See:41.6and41.7].

41.8.2

Core damage

Whenthecoreiscrushedseverely,itshouldbereplaced.Otherwisethespaceisfilledwithamixture
ofresinandmicroballoons.

41.8.3

Manufacture

The repairsequence fora sandwich panel with a damaged coredepends onwhether it isaccessible
from:

Oneside,or

Bothsides.

Ifthesandwichpanelisaccessiblefromonesideonly,theareaofdamagedcoreisremovedandapre
curedcompositeplate,bondedtoahoneycombplug,isthenfitted.Theskinisthenclosedbyatypical
flushrepair.
Figure41.8.1showsanexampleofasandwichpanelrepair.

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Figure41.81Sandwichrepair

41.9

References

41.9.1

General
[411]

M.Torres&B.Plissonneau
Repairofhelicoptercompositestructuretechniquesand
substantiations
AGARDConferenceProceedingsNo.402

[412]

Th.Thiele
RepairprocedureforcompositepartsontheAlphaJet
AGARDConferenceProceedingsNo.402

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[413]

AirbusIndustrie
A320:Structuralrepairmanual

[414]

R.H.Stone
Developmentofrepairprocedureforgraphite/epoxystructureson
commercialtransports
SAMPEMonographNo.1CompositeRepairs

[415]

G.Lubin
Handbookofcomposites
VanNostrandReinholdCompany,1982

[416]

J.F.Knauss&R.H.Stone
Demonstrationofrepairabilityandrepairqualityongraphite/epoxy
structuralsubelements
SAMPEMonographNo.1CompositeRepairs

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42
Basic characteristics of new advanced
materials
42.1

Introduction

The basic characteristics of the various groups of new advanced materials in ECSSEHB3220 are
described.Itservestohighlightreasonsforthedevelopmentofthedifferentgroupsofmaterialsand
the problems encountered in doing so. Information is presented and discussed in further detail in
subsequentchapters,including:

MetalsandMMCs

Technicalceramicsandceramicbasedtextiles

CMCs

Carboncarbon

Design aspects of the various material groups are given, along with examples of their actual or
intendedapplicationinspacestructures.
The majority of information is related to their hightemperature performance, gained from various
reusablevehicleconcepts.
Smarttechnologiesandthevarioussmartmaterialsarealsopresentedforspaceapplications

42.2

Material groups

42.2.1

Metallic materials

Information on more conventional and welldeveloped materials such as aluminium and titanium
alloysisnotgivenindetail.Theresumoftheircharacteristicsisusedasastartingpointforthenewer
developments,including:

Aluminium-lithium alloys,[See:Chapter46].

Dispersion strengthening

Powder metallurgy alloys

Superplasticalloys(SPF/DB)

Metalmatrixcomposites:

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Referenceismadetosourcedocumentsfortheestablishedalloysinaerospaceapplications.

[See:Chapter46foraluminium;Chapter47fortitanium]

42.2.2

Ceramic materials

42.2.2.1

General

Ceramicscanbebroadlygroupedas:

Reinforcingfibres,[See:42.6]

Monolithic, which is a large family of different materials also known as technical ceramics.
Theseareoftenproducedfrompowders,[See:Chapter43].

Fibrereinforcedcomposite,whicharethenclassedbythematrixphase,e.g.

siliconcarbide,[See:Chapter52]

glassandglassceramic,[See:Chapter53].

carbon,[See:Chapter54]

42.2.2.2

High temperature applications

Fibrereinforced ceramic composites and carboncarbon materials offer attributes for use in high
temperature applications; notably in propulsion and thermal protection systems. Significant studies
relatingtomaterialsdevelopmentandevaluationoccurredduringreusablespaceplaneprogrammes.

42.2.2.3

Dimensionally stable applications

Thelowthermalexpansioncharacteristicsofferedbymonolithicceramics,variousCMCsandcarbon
carbon composites have led to their evaluation for structures needing dimensional stability over a
widerangeoftemperaturesfromcryogenicupwards,e.g.supportsforopticalequipment,mirrorsfor
spacebasedtelescopes.

42.2.3

Material classification

42.2.3.1

High temperature capability

Materialscanbeclassifiedbygenerictype,e.g.polymer,metallicorceramicbased,[See:Chapter1],or
bytemperaturecapability,e.g.thoseofferingcapabilitiesabove600Candultimatelytowards2000C.
Figure42.2.1providesabroadindicationofultimatetemperaturecapabilities,whichcanbedefinedto
apointwherethematerialsareessentiallystable.Beyondthispointdegradationaccumulatesandthe
materialsresidualpropertiescanonlybeusefulforarestrictedduration.

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Temperature(C)

Figure42.21Classificationofadvancedmetallicandceramicmaterialswith
temperature

Figure 42.2.2 shows specific strength against increasing temperature for different materials. Other
thancarboncarboncomposites,whichshowincreasingstrengthwithtemperature,thetrendisfora
gradualstrengthreductionastemperatureincreasesandthematerialoptionsbecomemorelimited.

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Figure42.22Specificstrengthagainsttemperatureforadvancedmaterials

42.3

Features of alloys and metal matrix composites

42.3.1

Structural alloys

Theprincipalmetalalloysofstructuralinterestarealuminium,titaniumandthesuperalloys,notably
nickelbased. Supporting roles are provided by magnesium, copper, beryllium, intermetallics and
refractorymetals,Ref.[421],[422].
Alloys generally have a main constituent with additional alloying elements in varying proportions.
The alloy composition, its production route and its heat treatment and mechanical working history
determinethemechanicalproperties.
Examplesofcommonaerospacealloysinclude:

Aluminium[Seealso:Chapter46]:

2XXXSeries,e.g.2024(Copperprincipalalloyingelement)

7XXXSeries,e.g.7050(Zincprincipalalloyingelement)

Titanium[Seealso:Chapter47]:

Intermediatealphabeta,e.g.Ti6Al4V

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42.3.2

Properties

These alloys have good mechanical properties in their own right and are wellestablished, well
characterised materials which fulfil structural needs. However, the aerospace industries are always
seeking greater efficiency and longevity in structures from improved materials. This provides an
incentivetodevelopmetalalloysbeyondprecipitationandmechanicalhardening.
The material properties in which improvements are sought include, Ref. [423], [424], [425], [426],
[427]:

Greaterstrength,notably:

ultimatetensilestrength(UTS)

yieldstrength(YS)

Greaterstiffness

Highertemperaturecapability:

creepresistance

Betterfracturetoughness

Betterfatigueresistance

Bettercorrosionresistance

Optimisedthermalcharacteristics,e.g.

conductivity,

heatcapacity,and

dimensionalstability.

Therequirementsareusuallyapplicationdrivenandmaybeonlyafewselectedparametersfromthe
abovelistcanbeaddressedatonetime,itisimpossibletoimproveallsimultaneously.Whenattempts
are made to improve some parameters, there is a strong possibility that others are sacrificed or
reduced.
Allalloysareoptimisedtoenhancecertaincharacteristicsandabalanceorcompromiseisreachedon
arangeofengineeringproperties.

42.3.3

Material developments

Themeansofimprovingalloysorpreparingcompositesare:

Fineparticledispersions:

particlesize:submicrometre(<1m).

particletype:e.g.oxides.

particlevolumefractions:1%to9%,typically.

usuallyclassifiedas:
o

dispersionstrengthened(DS),or

mechanicallyalloyed(MA).

Discontinuousorparticulate reinforcedComposites(MMCs):

particlesize:Micrometrerange(1to50m).

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reinforcementisachievedbytheadditionofceramicparticles,e.g.:
o

siliconcarbide,

alumina,

boroncarbide.

ParticlefractionswithinMMCs:10%to20%,typically.

Continuousfibreorfilamentreinforcedcomposites(MMCs):

Fibrediameter:8mto200m.

Analogous to fibre reinforced plastics but with a metal matrix providing significant
strengthandstiffness.

FibrevolumefractionswithinMMCs:30%to50%,typically.

42.3.4

Effects of reinforcements

Theadditionofparticlesandfibreshasadisruptingeffectonconventionalalloymicrostructuresand
theusualprecipitationandgraincharacteristicsofsolidifyingmetalmelts.Asthevolumetriccontent
of reinforcement increases, the disruption becomes more acute and the chance of deleterious effects
increases. As reinforcement contents increase, the most obvious property to diminish is overall
materialductilityintermsofplasticdeformation,elongationtofailureandreductioninarea.Thiscan
presentuncertaintytodesignersandengineerswhoexpectoranticipatemetalstohavehighductility.
Dispersionstrengthened and particlereinforced metals are treated as isotropic materials. Fibre
reinforced MMCs are anisotropic and are considered as a group of materials in their own right
possessing property characteristics different from those of both metal alloys and fibrereinforced
plastics.
Low strains to failure (<1%) and lack of ductility are features of CFRP, MMC, intermetallic and
ceramic materials. As the number of applications of these materials increases, design experience is
beingaccumulatedwithlowstraintofailurematerials.

42.3.5

Processing

In preparing metal matrix composites, a wide range of reinforcing materials has been tried with an
equally large number of matrices. Only a small proportion of these have reached commercial
maturity.Thetwomainareasrequiringattentionare:

Costeffective production techniques for combining molten matrix with the reinforcement to
giveacontrollableandreproduciblecompositeproduct.

Optimum compatibility between matrix and reinforcement to ensure that both function in
unisontogiveacompositewithenhancedproperties.

The combining of molten metal with a large volume fraction of reinforcement is not without
difficulties. The interface between the two phases has considerable importance and a balance is
reachedoninterfacialbonding.

Verygoodbondingusuallyresultsfromadirectchemicalreactionproducing:

fibredegradation,

brittlefracturecharacteristics,and

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modestcompositestrength.

Verypoorbondingleadsto:

lowinterfacialshearstrengths,

lack of utilisation of reinforcement properties resulting in poor cohesion between fibre


andmatrix.

42.4

Features of ceramic and inorganic composites

42.4.1

Features

42.4.1.1

High temperature

For some space applications there is a need for materials which can provide a load bearing and
structuralfunctionathightemperatures,i.e.800Cto>2000C.

42.4.1.2

Materials

The materials are principally inorganic (nonmetallic) and ceramic compositions. In view of the
structuralimplications,materialswithbenignandprogressivefracturecharacteristicsarepreferredto
monolithic,brittlematerials,[See:Chapter43forconventionalmonolithicceramics].
Theconcentrationisonfibrereinforcedmaterialswithamatrixofeither:

Glass,

Glass-ceramic,or

Ceramic.

Carboncarboncompositesalsooffersomeuniquecapabilities.

42.4.1.3

Fracture

Composites achieve their benign fracture characteristics by ensuring that the matrix is decoupled
fromthefibres.Thisprovidesalargeinterfaceareawhichactsasacrackstoppingmediumandallows
fibre slippage and pullout. In many respects the composites can be viewed as rigidised fibre
(insulation) materials where sufficient integrity is provided for the composite to be classified as an
engineeringmaterial.
Themicrostructuresofthesecompositesarecomplexandthematrixatanytimecontainsasignificant
population of microcracks and microvoids. An optimised composite gives an element of pseudo
ductilityandfailswithnoticeablefibrepullout.
A monolithic ceramic has a nominal fracture toughness of approximately 4MPam1/2, a good
compositeisusuallyinexcessof15MPam1/2andpreferably30MPam1/2.
Thetermgoodcompositeindicatesamaterialwhichshowstolerancetothermalshockandthermal
cyclingandcansustainmicrocrackingandminorimpactdamagewithoutcatastrophicfailure.

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42.4.2

Properties

Mechanical strengths are modest (100MPa to 400MPa), but these are retained at high temperatures.
Ultimatefailurestrainscanbeintherangeof0.4%to1.0%,comparedwith0.2%orlessformonolithic
ceramics. Carbon fibrereinforced carbon possesses characteristics which are suited to high
temperature applications. Its excellent thermal stability is retained at temperatures approaching
2000C and is unique in that strength increases as the temperature rises. This is found in both the
pyrolysedmatrixandthefibres.

42.4.3

High-temperature use

42.4.3.1

Oxidation

Carboncarbon composite would be ideal for most applications were it not for its poor oxidation
resistance at temperatures exceeding 500C. For prolonged use in oxidising environments, elaborate
coatings and protection systems are used to give high thermal stability and hightemperature
synthesis,withprocesstemperaturesbetween1500Cand2000C,isnecessary.
Otherceramicmatrixcompositesofferhightemperaturestabilitywithouttheoxidationproblemsor
theveryhighsynthesistemperatures.Inthistherearevaryingdegreesofsuccess,influencedbythe
followingfacts:

Allceramicoxidationresistantfibres,suchassilicon carbideoralumina,showincreasingthermal
degradationandperformancelossattemperaturesbeyond1200C.

The most successful decoupling interface material between fibre and matrix is carbon which
performsthemechanicalrequirementsbutispronetooxidisation.

Progressively reducing the process temperatures, e.g. from ceramic (silicon nitride, 1500C) to
glassceramic (LAS, 1100C) to glass (borosilicate, 800C) equally reduces the maximum use
temperature.

Avoiding mechanical damage of the fibres during processing favours lowpressure, reactive
consolidationtechniques,butthesetendtoleaveresidualporosity(approximately10%).

Highpressureconsolidationeliminatesporositybutposesseverelimitationsoncomponentsize
andcomplexity.

42.4.3.2

Prolonged exposure

Above1000C,thecompositionandmicrostructureofceramiccompositescanundergochemicaland
diffusionreactions.Timeandtemperaturearethedeterminingparametersfordeleteriouscomposition
changestoreachsignificantproportionsanddegradethematerialbeyondanacceptablepoint.

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42.5

High temperature and interface phenomena

42.5.1

Effects of processing temperature

42.5.1.1

Metal and ceramic composites

In fibrereinforced plastics, the fibres are stable and inert at the processing and operating
temperatures. It is only the polymer matrix that chemically responds to its environment; it cannot
chemicallyreactwiththefibres.
Formetalsandceramicstheprocessingandoperatingtemperaturesarefarhigher,greatlypromoting
chemical reactions. Molten metalsare aggressiveand the largesurfacearea of fibre is susceptible to
damage. Therefore processing with molten metals needs to be accomplished as quickly as possible.
Ceramic processing also involves chemical reactions and diffusion mechanisms for matrix
consolidation,e.g.:

Sintering,

Polymerpyrolysis,or

Chemicalvapourdeposition,(CVD).

Allofthesemethodsrelyoncontrollingthedesiredreactionsandlimitingthedeleteriousones.Some
exampleswheredeleteriousreactionshaveneededcontrollingare:

Carbonfibrereinforcedaluminiumalloys:Ifmoltenaluminiumremainsincontactwithcarbon
fortoolong,thebrittlecarbide,Al3C4,forms.Thisoccursonthefibresurface,severelydegrades
the fibre, and causes a brittle interface. Carbon and aluminium also have an electrochemical
potentialdifferencewhichcancauseinternalgalvaniccorrosionunderhotwetconditions.

Silicon carbide Fibre Reinforced Aluminium Alloys: Very severe fibre degradation occurs if
molten aluminium is kept in contact for too long, i.e. more than a few minutes. The SiC is
convertedtoaluminiumcarbide.AmorecompatiblechoiceforaluminiumisAlumina(Al2O3).

Siliconcarbidefibreorfilamentreinforcedtitaniumalloys:Placingsiliconcarbideintomolten
titaniumleadstotitaniumcarbideformationproducingfibredegradationandabrittleinterface.
Only large diameter filaments can survive this, and then only if the fibres are coated with
titaniumdiboride(TiB2)orfibreswithacarbonrichsurface.

Tungstenfibrereinforcednickelsuperalloys:Tungstenissolubleinmoltennickelgivingbrittle
interfaces. A coating of thorium oxide (ThO2) acts as a diffusion barrier to control the
degradation.

42.5.1.2

Intermetallics

As confidence grows in using brittle materials, attention has been given to some which have
traditionallybeenclassifiedasundesirablewhenunintentionallypresentinconventionalalloys.These
include the intermetallics, notably titanium aluminide (Ti3Al) and nickel aluminide (Ni3Al). In their
pureform,theyarenotusableowingtobrittleness.
Bydopingandmicroalloying,greatimprovementscanbemadeto:

Ambientductility,

Hightemperaturestrengthretention,

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Reductionofoxidationembrittlement,and

Improvementofcreepresistance.

This effectively creates a new group of materials and can be taken a step further by using
intermetallicsasthematricesforcomposites.
The reinforcement of Ti3Al with niobium (Nb) coated silicon carbide fibres has been studied. The
niobium is selected as the interface to prevent a chemical reaction between the matrix and fibre.
EquallyitisadesirablemicroalloyingelementwithTi3Alforimprovingductility,soitsdiffusioninto
thematrixshouldnotbeahindrance.

42.5.2

High-temperature applications

42.5.2.1

Hydrogen-containing environments

Inhightemperatureapplications,notablypropulsionandthermalprotectionsystems,thepresenceof
hydrogenoxygen fuel in the former and oxygen in the latter pose problems. The small size of
hydrogenions,atomsandmoleculesmakesdiffusionrelativelyeasywithinmaterials,notablymetals,
manifesting itself as unacceptable material embrittlement. This causes concern for the integrity and
longevityoffueltanks,pipelines,pumpsandmotors.

42.5.2.2

Oxygen-containing environments

The presence of oxygen at high temperatures always causes concern because there is a natural
inclinationforallmetalstoformoxides.Insomecases,thisisadesirablemechanismforpassivating
thesurfaceofmaterialstorenderfurtheroxidationimpossible.Classicexamplesinclude:

AlAl2O3,

SiCSiO2

AlNAl2O3

Forexposedcarboncarboncomposites,oxidationisprogressiveandultimatelycatastrophic.
Given that materials oxidise, it is usually the case that oxidation should be controlled or inhibited.
Thisisusuallydoneby:

Carefulmaterialselection,

Avoidingmaterialconstructionswhich,underthermalcycling,produce:

spalling,

porosity,

cracking,or

delamination.

useofprotectivecoatings,ifnecessary.

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42.5.2.3

Temperature variations

Athightemperaturesmaterialsarerarelyusedunderisothermalconditions,i.e.therearealwayssome
heating and cooling cycles. Three phenomena contribute in determining the life expectancy of
materialsundernonisothermalconditions:

Thermal fatigueorthermalcycling:Cycliceventshaveacumulativeeffect.Materialexpansionis
similartomechanicalloading(fatigue)causinginitiationandpropagationofdamage.

Thermal shock: Heating rate and localised temperature rises affect materials. Uneven heating
givesrisetointernalstressesduetodifferencesinexpansion.

Coefficient of thermal expansion and material matching: Within a composite material, different
phasescanhavedifferingexpansioncoefficients.Differentmaterialswithinajointoracoating
and substrate can have different expansion coefficients. If these are heated over a wide
temperature range, the internal stresses can become very high. Stress relief usually occurs
through microcracking, spalling or even total fracture. Therefore, close CTE matching is
beneficialifalargetemperaturerangeisexpected.

42.6

Refractory and ceramic fibres

42.6.1

Introduction

42.6.1.1

General

Refractoryandceramicfibrescanbeusedas:

Reinforcementsincomposites,e.g.:

Carbon(rayon,pitchorpan),[See:Chapter52;Chapter54]

Siliconcarbide

Alumina

Boron

Thermalinsulation,[See:Chapter99].

Numerous types of fibres have been considered for reinforcing various metal and ceramic matrix
phases. Those types which have been studied, primarily during the development of composites for
hightemperature applications, are summarised. The majority are continuous fibres, although some
whiskerreinforcementshavealsobeenconsidered.
Notallthetypesoffibresdescribedarecommerciallyavailableorhavebeensuccessfulincomposite
manufacture.

42.6.2

Types of refractory and ceramic fibre

Table42.6.1identifiesrefractoryandceramicfibreswhichcansustaintemperaturesof1000Cormore
andindicatestheiruseincomposites.

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42.6.3

Use in composites

Themajorityofsuccessfulcompositedevelopmenthascentredon:

Highstrengthcarbonfibres

NicalonSiCfibres

Allcommerciallyavailablereinforcingfibres,exceptcarbon,tendtodegradeprogressivelyintermsof
strengthattemperaturesbeyond1200Cto1300C.Propertiesarethenamatterofassessingresidual
strengthsandwhetherthesearesufficienttobeuseful.

Table42.61Reinforcingfibresavailableforuseininorganiccomposites
Fibre

Status

HST300

Nicalon
Tyranno
SCSfilaments
Derivatives:
MPDZ
HPZ
MPS
Fiberamic

Comments
Carbon
Excellentmechanicalproperties[See:Chapter2],withstabilityto
2000C+,butwilloxidise.
SiliconCarbide
Basedonfibrepyrolysis.Goodhandleability&tensilestrength.
Significantpropertylossabove1200to1300C.
Goodthermalstability,butavoidedasdifficulttoprocess.

LessthermallystablethanNicalon/Tyranno.Goodhandleability.
Applicabletoalimitednumberofmatrixmaterials,mainlyglass
ceramics.

Underdevelopment,notyetavailable.
Alumina

FiberFP
Safimax
Saffil
ALMAX
Sumitoma
DENKA
Nextel312
Nextel440
Nextel480
PRD166
ZicarZYF100

Aluminafibreswithgoodthermalstability,butbrittlewithmodest
strength.Usefulpropertiesto1500C.

Modifiedaluminafibreswithbettertensilestrengththanhigh
alumina,butwithreducedthermalstability~1400C.

Littleknown
Boron

Boron
Borsic

Goodthermalstability,butavoidedasdifficulttoprocess.

Key:

Widelyused

Gaininguseinceramicandglassceramicmatrixcomposites

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42.6.4

Thermal stability

42.6.4.1

General

Thermalstabilityisoftengainedattheexpenseoftensilestrength,asinthecaseofalumina(Al2O3)
compared with silicon carbide (SiC). Table 42.6.2 gives details of the commercial fibres and some
underdevelopment.

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Table42.62ContinuousfibreandfilamentreinforcementsusedinMMCsandCMCs
Specific
Grade

Chemical
Composition
(%)

[Manufacturer]
CARBON
High Strength
grade.
e.g. Toray T300

> 99C

Density
(kgm-3)

1760

Fibre or
Filament
Diameter
(m)

Tensile
Modulus
at RT
(GPa)

235

Tensile
Strength
at RT
(MPa)

3500

Tensile
Strain to
Failure %

Product Forms
and
Availability

Comments

1.5

Yarn and fabrics widely


available. Can be
braided.
Net-shape preforms,
(multi-directional).

Carbon fibres possess excellent thermal


stability but will oxidise at low temperatures.
They are used with carbon and silicon
carbide matrices for high temperature
applications.

3 grades of yarn
available.
Limited standard
fabrics.

Used in MMCs and CMCs.


Stable to 1200C, but will gradually lose its
properties as temperatures > 1500C to
1600C. Grade NL200 specific to CMCs
CVD fibre has good thermal stability. Used
in MMCs but not CMCs. It Is difficult to
process and tends to be avoided.
SiC fibre contains titanium and oxygen and
is relatively new (1987) and untried.
Combines well with aluminium alloys but
untried for CMCs

SILICON CARBIDE
Nicalon
(Nippon Carbon)

54.3Si, 30C, 11.8O


(-SiC)

2550

15

196

2740

1.4

SCS Filaments
(AVCO, USA)

-SiC deposited by CVD


on carbon fibre substrate

3300

140

427

3450 +

0.81

Si-Ti-C-O:
44.2Si, 24.5C, 11.0Ti,
12.3 O
(-SiC + TiC)

2300

8-12

200-220

2800-3000

1.4-1.5

2300
2350
2600 2700

10-15
10
10-15

175-210
140-175
175-210

1750-2100
2100-2450
1050-1400

0.8-1.2
1.2-1.7
0.5-0.8

15

220

1800

>99 -AI203

3950

20

380

85AI203.15SiO2

3200

9-17

95 -AI203

3300

96-97AI203

3300

Tyranno
(UBE, Japan)
MPDZ
HPZ
MPS
(Dow Corning/
Celanese, USA)
Fiberamic (RhonePoulenc, France)
ALUMINA
Fiber FP
(Du Pont)
Alumina
(Sumitomo, Japan)
Safimax SD
Saffil RF/RG (ICI)

47Si, 30C, 15N, 8O


59Sl, 10C, 28N, 3O
69Sl, 30C, 1O
?

Continuous filament.
Cannot be woven.

Development product.

Variants of SiC compositions. MPS likely to


have the highest thermal stability.

1.2

Development fibre
Not yet available.

Under development in conjunction with SEP


for use in MMCs and CMCs

1380

0.4

Yarn from Du
Pont(USA). Special
fabrics possible.

210-250

1800-2600

0.7-1.2

300

2000

0.67

Uncertain

300

2000

0.67

Bulk and matted fibre

Good thermal stability and is almost pure


alumina.
Very brittle and tends to be avoided.
Adding silica improves strength but lowers
thermal stability.
Small diameter fibre, untried in CMCs
Principally an Insulating fibre which can be
used in some MMC composites.

Little known.

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Specific
Grade
[Manufacturer]
ALMAX
[Mitsu mining Co.
Japan]
Specific
Grade

Chemical
Composition
(%)
99.5AI203
-alumina
Chemical
Composition
(%)

[Manufacturer]
ALUMINA - continued
DENKA (Japan)
80AI203, 20Si02
Continuous
Alumina
80 -AI203 20 stabilised
PRD-166
(Du Pont)
ZrO2
ALUMINA-BORIA-SILICA

Density
(kgm-3)

Fibre or
Filament
Diameter
(m)

Tensile
Modulus
at RT
(GPa)

Tensile
Strength
at RT
(MPa)

3900

10

330

1800

Density
(kgm-3)

Fibre or
Filament
Diameter
(m)

Tensile
Modulus
at RT
(GPa)

Tensile
Strength
at RT
(MPa)

3100

10

170

1700

1.0

Various yarn and fabric


forms available.

4200

20

380

2070

0.6

Development product in New fibre yet to be released.


Du Pont (USA).
Improved strength on Fiber FP.

2700
3050
3100

12
12
12

152
186
220

1720
2000
1900

1.13
1.07
0.86

Origin USA. A range of


yarns and fabric
available as standard
products.

Modified alumina-silica fibres that provide a


compromise between strength & thermal
stability. Used in MMCs and CMCs.
Property loss >1300C.

Little known.

Tensile
Strain to
Failure %

Product Forms
and
Availability

Various product forms


available including
yarn and fabric.
Tensile
Product Forms
Strain to
and
Failure %
Availability
0.5

Comments

No information as yet on the use in


composites
Comments

No information as yet on use in composites.

Nextel 312
Nextel 440
Nextel 480 (3M)

62AI203,14B203, 24Si02
70 AI203, 2 B203, 28Si02
70 AI203, 2 B203, 28Si02

ZIRCONIA
Zircan
ZYF-100 (USA)

Stabilised ZrO2 with HfO2


and Y203

5600 5900

4-6

CVD deposited boron on


tungsten wire substrate

2470 2580

101-203

400

3500

0.88

Continuous filament.
Cannot be woven

Good thermal stability, but brittle and


difficult to process.

SiC coated boron on


tungsten wire

2380 2610

101-203

400-414

2760

0.66-0.69

Continuous filament.
Cannot be woven

Good thermal stability, but brittle and


difficult to process.

BORON
Boron Filaments
(AVCO)
BORSIC
Borsic Filaments
(USA)

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42.6.4.2

Silicon carbide fibres

Figure42.6.1,Figure42.6.2andFigure42.6.3showthefibretensilestrengthatvarioustemperatures,
fortwogradesofNicalonfibre,Ref.[4210].

Afterheattreatmentsinflowingwetairfurnaceenvironment(12hoursoak)

Figure42.61SiCNicalonfibretensilestrengthatelevatedtemperature

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Afterheattreatmentinflowingargonfurnaceenvironment(12hoursoak)

Figure42.62SiCNicalonstandardgradefibretensilestrengthatelevated
temperature

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After12hourfurnacesoakinflowingargon

Figure42.63SiCNicalonceramicgradefibre:tensilestrengthatelevated
temperature

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The tensile strength of Nicalon fibres after prolonged exposure at various temperatures is shown in
Figure42.6.4andFigure42.6.5,Ref.[4211].

Figure42.64SiCNicalonfibre:tensilestrengthafterhightemperatureexposure
inair

Figure42.65SiCNicalonfibre:tensilestrengthafterhightemperatureexposure
inargon

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ThehightemperaturetensilestrengthandstiffnessofTyrannoandNicalonSiCfibresarecomparedin
Figure42.6.6andFigure42.6.7,Ref.[4212].

Figure42.66SiCfibresNicalonandTyranno:tensilestrengthatelevated
temperature

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Figure42.67SiCfibresNicalonandTyranno:modulusatelevatedtemperature
42.6.4.3

Alumina-based fibres

Figure42.6.8andFigure42.6.9comparethetensilestrengthandmodulusofthreegradesoffibreat
elevatedtemperatures,Ref.[4212].

Figure42.68Aluminafibres:tensilestrengthatelevatedtemperature
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Figure42.69Aluminafibres:modulusatelevatedtemperature

TheeffectofahightemperaturetreatmentisshowninFigure42.6.10foraluminabasedfibresPRD
166 and FiberFP. The stability of the two fibres after exposure to high temperatures is shown in
Figure42.6.11,Ref.[4213].

Figure42.610Aluminafibres:tensilestrengthagainstexposuretoelevated
temperature

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Figure42.611Aluminafibres:tensilestrengthagainstexposuretime

Figure 42.6.12 and Figure 42.6.13 show the hightemperature strengthstiffness stability of Alumina
BoriaSilicaNextelsinglefilaments,Ref.[4214].

Figure42.612Aluminaboriasilicasinglefilament:tensilestrengthatelevated
temperatureinair

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Figure42.613Aluminaboriasilicasinglefilament:tensilemodulusatelevated
temperatureinair

42.6.4.4

Whisker reinforcements

Combinedhighthermalstabilityandhighstrengthhastoanextentbeenachievedwithwhiskers,e.g.
high purity, stoichiometric, SiC whiskers. The problem is then to keep this good combination in a
composite. To date, this has been far from successful because chemical reactions degrade the very
smalldiameter(~1m)whiskers.

42.6.4.5

Thermal expansion

Thermal expansion is an important characteristic of refractory composites. It should be similar for


bothfibreandmatrix.
Figure42.6.14andFigure42.6.15givestiffnessandCTEvaluesforsomefibresandmatrices.

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Figure42.614Modulusforvariousfibresandmatrixmaterials

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Figure42.615Coefficientsofthermalexpansionforvariousfibresandmatrix
materials

42.7

References

42.7.1

General
[421]
NOTE

MILHDBK5F:MetallicMaterialsandElementsforAerospaceVehicle
Structures.November1990
ReplacedbyMMPDS01,Ref.[4215]

[422]

MetalHandbook
ASMInternational,10th.Edition,Volume2
ISBN0871703785(V.2),1990

[423]

M.Taya&R.J.Arsenault
MetalMatrixCompositesThermomechanicalBehaviour
PergamonPress.ISBN0080369839,1989

[424]

W.S.Johnson
MetalsMatrixCompositesTesting,AnalysisandFailureModes
ASTMSTP1032,ISBN083011270X.1989

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[425]

J.Fulleretal
DevelopmentsintheScienceandTechnologyofCompositeMaterials
ECCM4,September2528,1990,ISBN1851665625

[426]

SymposiumonHighTemperatureComposites
ProceedingsoftheAmericanSocietyforComposites.June1989
TechnomaticPublishingCompany.ISBN877627002

[427]

S.G.Fishman&A.K.Dhingra
CastReinforcedMetalComposites
ConferenceProceedings.ASMInternational,September1988
ISBN0871703394

[428]

AnnualConferencesonCompositesandAdvancedCeramicMaterials
PublishedbyAmericanCeramicSociety
11th.AnnualConference,January1823,1987.ISBN01966219

[429]

K.S.Mazdiyasui
FibreReinforcedCeramicCompositesMaterials,Processingand
Technology
NoyesPublication,1990

[4210]

T.J.Clarketal
ThermalDegradationofNicalonSiCFibres
Proceedingsof9thAnnualConferenceonCompositesandAdvanced
Ceramics,p576588,1985,ACSpublication

[4211]

T.Ishikawaetal
Strength&StructureofSiCFiberafterHighTemperatureExposure
ProceedingsoftheSymposiumonHighTemperatureMaterials
ChemistryIV,theElectrochemicalSociety,Vol.885,p205217

[4212]

D.J.Pyscheretal
StrengthsofCeramicFibersatElevatedTemperatures
J.Am.Cer.Soc.Vol.72,No.2.p284288.(1989)

[4213]

J.C.Romine
NewHighTemperatureCeramicFiber
Ceram.Eng.Sci.Proc.,8[78]p755765(1987)

[4214]

A.R.Holtz&M.F.Grether
HighTemperaturePropertiesofThreeNextelCeramicFibers
32ndInternationalSAMPESymposium,April69,1987,p245256

[4215]

R.C.Riceetal.
MetallicMaterialsPropertiesDevelopmentandStandardization
(MMPDS)
DOT/FAA/ARMMPDS01,January2003
Website:www.hdbk5.battelle.org/milhdbk2.htm

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43
Technical ceramics
43.1

Introduction

43.1.1

General

43.1.1.1

Characteristics

Ceramic describes a large group of material compositions having diverse characteristics and
properties. Ceramics are available in a variety of forms, e.g. powders for consolidation, fibres and
whiskers of variouslengths and diameters, preconsolidated shapes (tubesand plates), andcustom
shapeditems.

[Seealso:42.6forceramicreinforcingfibresforcomposites]

Manytypesofceramicsaresuccessfullyusedinindustryforaverywidevarietyofapplications.They
aretypicallyemployedfortheirelectricalandthermalinsulation;electricalandthermalconductivity;
thermal stability; corrosion and wearresistance, or a combination of one or more properties. Some
types of ceramics are used for applications that make us of their characteristics, such as bearing,
friction and high stiffness. For extreme lowtemperature applications, low thermal expansion
encouragedevaluationofsomeceramicsforapplicationsdemandinghighdimensionalstability.

43.1.1.2

Terminology

Within the context of this handbook, technical ceramicsare monolithic materials, without deliberate
additions of fibrereinforcement, hence excluding ceramic matrix composites, [See: 52]. Another
means of distinguishing between monolithic and composite is that the mechanical properties of
technicalceramicsareusuallystatedonastatisticalbasis,i.e.Weibull.
Overtheyears,technicalceramicshavealsobeenknownas:

engineering ceramic or fine ceramic, in order to differentiate between those offering


characteristics suitable for engineering applications and other types used for construction
products,sanitaryware,tableware,fibrousinsulationproductsandrefractories.

advancedtechnicalceramic,whichwasadoptedafterextensiveresearchanddevelopmentinto
somenewmaterialslargelydestinedforaeroengines.

Althoughthetermsfineceramicoradvancedtechnicalceramicarestillusedinsomeorganisations,
technicalceramicisnowmorecommon,Ref.[431],[432].

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In addition to those types of monolithic technical ceramics used for industrial or engineering
applications,theotherdivisionsofceramicscommonlymadeare:

Electronictechnicalceramics:Althoughconstitutingalargeproportionofthetechnicalceramic
market,theyarenotconsideredasstructuralmaterials,e.g.chipcarriersanddevicesubstrates.

Coatings:Althoughmanytypesofceramicsareusedascoatingsappliedtosubstratematerials,
thesearenotincludedhere.Ceramiccoatingsareverycomplexmixtures,whicharetailoredto
provide protection of the substrate against a number of environments, e.g. hot corrosion,
chemical attack, erosion. Where ceramicbased coatings have been applied to substrate
materials described in this handbook, they are mentioned in that chapter, e.g. thermal barrier
coatingsonSuperalloys.

Functional ceramics are not included here, i.e. dielectric, piezo or pyroelectrical grades used
forelectronicdevicessuchassensorsandigniters.Somefunctionalceramicsareusedinsensor
systemsandactuatingdevicesforsmarttechnologies,[See:Chapter90].

Opticaldevices:Materialsusedsolelyforopticaldevicesarenotincluded,e.g.lenses,windows,
fibre optics, because their selection is usually made on their optical performance rather than
loadcarryingability.Someexamplesofmaterialsthatofferacombinationofopticalandload
bearingpropertiesaredescribedasspecialitymaterials,[See:43.16;43.17].

43.1.2

Technical ceramics for space structures

43.1.2.1

Materials

Thebasictechnicalceramicmaterialfamiliesofprimeinterestforspacestructuresare,[See:43.2]:

oxides,

carbides,

nitrides,

carbon(elementalcarbon)

glassceramics,alsoconsideredasstructuralglasses,e.g.commerciallyavailableproductssuch
asZerodurandULE.

43.1.2.2

Application examples

Until recently, monolithic ceramic materials were of low interest within the space community for
structural applications. In general, ceramics have the reputation of being brittle and intolerant of
shockandvibrationalloads.This,inpart,ledtothedevelopmentofCMCsforreusablespaceplane
technologies.
Low thermal expansion properties coupled with other inherent characteristics (electrical, optical or
environmental resistance) have provoked a new interest in the potential use of some technical
ceramicsinspace,particularlytomeetthedimensionalstabilitydemandsofsystemsoperatingatvery
highfrequency.
Massremainsadesigndriverforallspacecraft,leadingtointerestinlightweightceramicforms,such
asfoams,alongwithinnovativemassoptimiseddesigns,[See:43.18;43.19]
The wider use of ceramics is encouraged by a growing knowledgebase from applications in other
industrysectorsandalsobytheincreasingnumberofinternationallyrecognisedstandardsavailable,
e.g.fortesting.

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43.2

Material groups

43.2.1

Composition

All technicalceramics areessentiallysynthetic materials produced either from modified minerals or


by chemical processing. These wide ranges of materials tend to be grouped by their basic chemical
composition,i.e.:

Oxides

Carbides

Nitrides

Elemental,suchascarbon.

Structural Glasses And Glass-Ceramics

Each of the composition groups contains a variety of materials of different formulation. Some are
highpurity, single constituent grades whereas others are complex blends or chemical compounds.
Within a single family, materials provide a range of mechanical or physical properties for use in a
varietyofapplications.
Commercialceramicproductsaredescribedinanumberofways,i.e.:

Mineralorigin,e.g.steatite,

Chemicalformulation,e.g.magnesiumsilicate,

Molecularformula,e.g.MgOSiO2,

Manufacturersproductname.

Manufacturers usually offer several grades of the same basic ceramic, often classed by purity or
composition.
Forcompleteness,allcommontypesofcommercialtechnicalceramicsarelistedintablesbytheirbasic
chemical composition. Those with greyed backgrounds are of less interest for structural space
applicationsandarenotdiscussedfurther.

43.2.2

Oxides

Table 43.2.1 introduces some of the general features of common commerciallyavailable oxide
technicalceramics.Ofthese,materialsthatprovideausefulcombinationofmechanical,electricaland
thermal characteristicsare of interest for aerospace engineeringapplications,e.g. grades ofalumina,
silicaandzirconia.

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Table43.21Technicalceramics:Oxidesgeneralfeatures
OxideType

Alumina
Aluminium
oxide
Al2O3 [See:
43.6]

Features
High stiffness.
Hard and brittle.
Properties retained to about 800C,
but reduce significantly above
1000C.
Chemical resistance to both acid and
alkalis (except HF).
Excellent electrical insulation.
Medium shock and thermal cycling
resistance.

Beryllia
Beryllium oxide
BeO [See:
43.16]

Good chemical stability.


Excellent electrical insulator.
High thermal conductivity.
IR transparent.
Low thermal neutron absorption.

Cordierite
Magnesium
aluminosilicate
Magnesia
Magnesium
oxide
MgO

Moderate strength.
Good electrical insulation.
Low thermal expansion.
Moderate mechanical properties.
Poor thermal shock resistance.
High chemical resistance, including
molten metals.

Mullite
3Al2O32SiO2

Low mechanical properties.


Poor toughness.

Silica
Silicon dioxide
SiO2 [See:
43.11]
Steatite
Magnesium
silicate
MgOSiO2
Titania
Titanium
dioxide
TiO2
Zirconia
Zirconium
dioxide
ZrO2 [See:
43.14]
Key:

Excellent thermal shock resistance.


Translucent or transparent
depending on process route used.
Often a modified talc formulation.
Abrasives.
Dielectric properties.
High dielectric properties.
Wear resistance.
Blended with other oxides to
stabilise microstructural phases:
Fully stabilised.
Partially stabilised (PSZ), including
forms known as TZP tetragonal
zirconia polycrystal and TTZ
transformation toughened zirconia.

Comments
Zirconia additions (ZTA) improve
toughness and strength.
Synthetic sapphire is a single
crystal form of alumina; often used
for optical applications.
Translucent alumina is used for
high-temperature, optical
applications, e.g. lighting.
Alumina fibres are used as
reinforcement phase in metals and
ceramics.
Alumina-titanium carbide is used
for cutting tools.
Toxic.
Thermal management in
electronics-electrical.
Microwave applications, e.g.
windows and radomes.
Nuclear industry.
Porous types for catalyst supports.
Impervious types for electrical uses.
High-temperature refractory uses
(up to 2400C).
Single crystal forms for optical
uses.
Refractory material.
Toughness can be improved by
formulation and processing.
Fused quartz or vitreous silica for
optical uses.
Fused silica for thermal shock
resistance.
Grinding-cutting media.
Electronic-electrical uses.
Electronic applications.
Semiconducting type used as
electrodes or to discharge static
(process industries).
Fully stabilised materials are used
as refractories.
PSZ for thermal resistance. TZP for
high strength and TTZ for
engineering uses.
At high temperatures PSZ becomes
electrically conductive.

Greybackground:lessofinterestforspacestructuralapplications

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43.2.3

Carbides

Table43.2.2givessomegeneralfeaturesofcommerciallyavailablecarbidetechnicalceramics.Whilst
boroncarbidecanbeconsideredforparticularapplications,siliconcarbidehasarangeofpropertiesof
mostinterestforspaceapplications,[Seealso:43.12].

Table43.22Technicalceramics:Carbidesgeneralfeatures
CarbideType
Boroncarbide
B4C[See:43.8]

Siliconcarbide
SiC[See:43.12]

Features

Comments

Extremelyhard.
Lightweight.
Relativelygoodfracture
toughness.

Wearresistanceuses.
Impactresistance(armour).
Neutronabsorption.

Mechanicalpropertiesvarywith
theprocessingrouteused.
Thermalstabilitytoveryhigh
temperatures(2200Cto2800C,
dependingontype).
Hard.
Goodoxidationandhotcorrosion
resistance,dependingonpurity.
Impactresistance(armour).
Wearresistance.
Moderatethermalconductivity.
Moderateelectricalconductivity.

Variousprocessingmethodsused
togivearangeofmaterials(from
refractoriestoengineering
materials).
Usedfordimensionallystable
structuresinspacebasedand
terrestrialtelescopes.

43.2.4

Nitrides

Table43.2.3providessomegeneralfeaturesofcommerciallyavailablenitridetechnicalceramics.The
characteristicsofdifferentgradesarelargelyduetotheirprocessingmethods.

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Table43.23Technicalceramics:Nitridesgeneralfeatures
Nitridetype

Features

Highthermalconductivity.
Aluminiumnitride Goodelectricalinsulation.
AlN[See:43.7]
Powderspronetomoistureuptake
affectingelectricalproperties.

Comments
Thermalandelectricalproperties
dependonpurity.
Heatmanagementinelectronic
applications.
Windowsforvisibletoinfrared
systems.
Hexagonal(powders)usedas
hightemperaturesolidlubricant.
Densifiedshapesforinsulators
andhightemperaturerefractories
ininertatmospheres.
Cubicformusedforabrasives.

Boronnitride
BN[See:43.9]

Microstructuredeterminesproperties:
Hexagonalformsimilartographite.
Propertiesareanisotropic.Oxidisesin
airabove800C.
Cubicformisextremelyhard.

Siliconnitride
Si3N4[See:43.13]

Goodcreepresistance.
Goodthermalshockresistance.
Highstiffness.
Lowthermalexpansion.
Notelectricallyconductive(pure).
Hightemperaturestrength(1500Cin
vacuum;disassociatesat1850Cin
nitrogen)dependsonprocessingused:
RBSNreactionbondedsiliconnitride
orreactionsintered:porous,
moderatestrengthbuthighthermal
shockresistance.Modifiedprocessing
forfine,evenporositytoimprove
strength.
Hotpressedorhotisostaticpressed
materials:veryhighstrengths,good
fracturetoughnessandoxidation
resistance(to1200C).Creepresistance
dependsonsecondary,glassyphases.
Sinteredmaterials:strengthscan
approachhotpressedvariants.
Modifiedcompositionscanincrease
toughnessattheexpenseofstrength.

Strengthpropertiesdependon
processingmethod.
RBSNvariantsareusedfor
refractorytypeapplications.Non
wettingbymoltenmetalsenables
usesinmetalandprocess
industries.
Hotpressedorisostaticpressed
areusedforhightemperature
engineeringcomponents,e.g.gas
turbineandengineparts.
Sinteringenablesproductionof
shapedpartsnotpossiblebyhot
pressing,butcancompromisea
levelofmechanicalperformance.

Highstrength.
Goodfractureresistance.
Excellentwearresistance.
Goodthermalshockresistance.

Hightemperaturewear
applications,e.g.engines
(combinedmechanicalproperties
andhardness).Alsousedfor
cuttingtoolsandweldingjigs.
Conductivesialonsareblended
withcompoundssuchastitanium
carbide.

Sialon
Siliconaluminium
oxynitride

Key:

Greybackground:lessofinterestforspacestructuralapplications

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43.2.5

Elemental

43.2.5.1

Carbon

Carbonisusedinitselementalformsandcanbeclassedasatechnicalceramic.
CarbonmaterialsareerroneouslyknownasgraphiteintheUSA.Inthecontextofthishandbook,the
termgraphiteisusedonlyforthesoft,hexagonallycrystallised,allotropeofcarbon.
Carboncanhaveawiderangeofpropertiesdependingonitsstructure,fromtheextremehardnessof
diamond(naturalorsynthetic)toglassyamorphousformsandsoftgraphites,[See:43.10].
Comparedwithothertechnicalceramicgroups,carbonshave:

Moderate mechanical properties can be retained to about 3000C in inert or reducing


atmospheres. In oxidising atmospheres and air, the upper limit is governed by the oxidation
rate. This in turn is heavily influenced by the microstructure, hence: graphite (anisotropic),
400C; lower for amorphous or crystalline carbons (isotropic). The upper use temperature is
looselydefinedasthepointatwhichoxidationratesbecomeexponential.

Goodelectricalconductivity,

Moderatethermalconductivity,

Goodthermalshockresistance.

Table43.2.4summarisessomefeaturesofcommerciallyavailablecarbontechnicalceramics.
Themajorityofcarbonbasedstructuralcomponentswithinspacevehiclesarecomposites,however,
somediscretecomponentsmadefromcarbontechnicalceramicshaveflown,e.g.componentsinSpace
ShuttleandISS,suchassealsandbearings,Ref.[433].
Foams destined for structural roles are a recent innovation, e.g for spacecraft thermal management
systems,[See:43.10]

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Table43.24Technicalceramics:Carbonsgeneralfeatures
CarbonType

Graphite [See: 43.10]

Features
Solid:
Soft, weak material.
Self-lubricating properties.
Anisotropic properties.
High temperature and corrosion
resistance.
Porous:
Exfoliated (graphite foil in USA).
Foams.

Vitreous carbon

Carbon-Graphites
(mechanical carbons)
[See: 43.10]

Pyrolytic carbon
[See: 43.10]

Non-porous, amorphous glassy


form created from the thermal
decomposition of a carbon-rich
material, e.g. resins, pitch, tars.
Combined strength and corrosion
resistant.
Combination of amorphous
carbon and graphite.
A proper mixture of the two
materials is strong and hard
with a low friction coefficient.
Excellent corrosion resistance.
Can operate at temperatures
above 315C for extended periods
of time (depends on grade).
Anisotropic properties.
Higher strength compared with
conventional polycrystalline
graphite.

Siliconised carbon

Compared with carbon alone:


Increased hardness.
Lower porosity.
Improved oxidation resistance.

Fibres
[See: Chapter 2;
42.6]

Most common reinforcing fibre


for advanced composite
materials

Diamond
[See: 43.17]

Extremely hard.
Abrasion and wear resistant.
Developments in synthetic
process techniques now enable
large, simple shapes to be
manufactured rather than just
thin films or coatings deposited
on substrates.

Key:

Comments
Lubricants for high or low
temperatures.
Anisotropy can be controlled by
processing.
Refractories and process
industries.
Flexible sheet for gaskets and
seals.
Thermal management systems.
Constituent of refractories, used
as a binder matrix phase for other
materials, e.g. carbon, graphite
and SiC; especially carbongraphites (mechanical carbons).
Specialist uses only, e.g.
laboratory equipment.
Materials can be created to
achieve a balance of properties,
i.e. range of mechanical carbon
materials for a variety of wearresistant uses, e.g. bearings,
seals, pumps.
Produced by deposition onto
substrates, often from chemical
vapours, e.g. CVD process.
Silicon carbide surface layer
formed by liquid or vapour
infiltration processes. Processes
adapted and improved for ceramic
composite manufacture, [See also:
Chapter 89].
Wide variety of fibre properties
and characteristics depending on
processing methods and
treatments.
Abrasives and cutting tool
industries.
Wear protection (coatings and
films).
Optical applications.
Thermal management.

knownassiliconizedgraphiteintheUSA;Greybackground:lessofinterestforspace
structuralapplications

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43.2.6

Glass-ceramics

Glassceramics,also known as structural glasses,are a group ofmaterials that containabout 70% to


100%crystallinephaseswithinaglassymatrix,[See:43.15].
Themainfeaturesinclude:

Highstrength.

Lowthermalexpansion.

Goodthermalshockresistance.

Goodcorrosionresistance.

Goodwearresistance.

Electricalinsulation.

Gooddielectricproperties.

Commerciallyavailable compositions are generally tailored to optimise particular properties, e.g.


extremelylowthermalexpansionormachinability,[See:43.15].
Characteristicsofinterestforspaceusearelowthermalexpansionfordimensionallystablestructures
combinedwithdielectricorelectricalinsulation,e.g.forantennastructures,[See:43.15;43.19].

43.2.7

Sources

There are numerous manufacturers and suppliers of technical ceramics worldwide. Manufacturers
usuallyofferacomprehensiverangeofmaterialtypesandawiderangeofgradesforanyparticular
material.Theyusuallyalsoprovideacomprehensivedesigndevelopmentandprocessingservicefor
theirmaterials.Ingeneral,commercialproductshaveevolvedovermanyyearsasapplicationsmoved
from refractories to electronics and structural engineering applications. In recent years, some of the
largercompanieshavebeenactiveinacquiringorcreatinglicensingordistributionagreementswith
other organisations to enhance their product ranges, e.g. Boostec and CoorTek for silicon carbide in
spaceapplications.
Technical ceramics continue to be used mainly for some combination of their hightemperature,
corrosion resistance and electrical characteristics, so available property data corresponds to these
prime markets. For example, it is rare to have data on lowtemperature performance from
manufacturers.
Speciality materials, such as optical grade materials and glasses, tend not to be supplied by
mainstreamtechnicalceramiccompanies.
Table 43.2.5 summarises some examples of sources of commercial materials, including those
providing specialist product forms, e.g. foams, [See also: Chapter 26 for foam cores in sandwich
panels].

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Table43.25Technicalceramics:Sourcesexamples

Boostec (F)
Bettini (I)
Carbon Lorraine (F)
Carpenter (USA)
Ceradyne
CeramTech

ECM (D)

Element Six (3) (UK, NL)

ERG Aerospace (USA)

Fraunhofer IKTS (D)

GE Advanced Ceramics
Graphite Metallizing
(USA)
HITCO (USA)

Kubota

Kyocera

MER Corp. (USA)


Morgan Group (2) (UK)
NGK
POCO Graphite Inc.
(USA)
Precision Ceramics
Safran Group - Snecma
(F)
Schott (D)
SCT (F)

Schunk (D)

SGL (D)

St. Gobain (1) (F)


Toshiba Ceramics
TRL - Touchstone
Research Lab. (USA)
Ultramet (USA)
Key:

Speciality

Corning Corp.
Dynamic Ceramic (UK)

Glass
ceramics

Zirconia

Silicon
carbide
Silicon
nitride

Silica

Carbon

Boron
carbide
Boron
nitride

Cercom
CoorsTek

Aluminium
nitride

Source(4)

Alumina

Typesoftechnicalceramics

(1)St.GobainincludesformerproductsofNorton,AnnaWerk,Cesiwid,Carborundum;(2)Morgan
groupincludesMorganAdvancedCeramics,MorganAdvancedMaterials&Technology,
Haldenwanger,MorganPerformanceMaterials;(3)FormerlyDeBeers;(4)Sourcesare
indicativeonlyandnotanexhaustivelist.

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43.3

Design aspects

43.3.1

Guidelines

43.3.1.1

General

Compared with conventional engineering materials, ceramics are brittle and this inherent feature
should be taken into account in the design approach used, [See also: 43.15 design with glass
ceramics].
Historically, selection of technical ceramics for engineering applications was based on thermal or
electrical performance needs first and then the ability to resist any mechanical loads arising. In
demanding hightemperature environments, this meant that technical ceramics were only applied
beyondthecapabilitiesofconventionalmaterials.Forelectricalinsulationapplications,useofmetals
isimpossible,soceramicswereusedwhereplastics(wheninvented)lackedadequateperformance.
Overrecentyears,agrowingimpetusfortheuseoftechnicalceramicsinmainstreamapplicationshas
helpedincreasetheirknowledgebase,e.g.standardsforpropertyevaluation,morereliableproperty
data, improved processing and availability of design tools. These can now be applied to the more
demanding,highperformanceindustrysectors,suchasaerospace.

43.3.1.2

Material and process selection

Theirinherentbrittlefracturebehaviour,andtheconsequencesofthisfailuremode,makethespace
industrywaryofceramicsandglasses.Therefore,allaspectsofselection,designandverificationare
subjecttoreviewandapprovalbythefinalcustomer,[See:ECSSQ7071].
Other than applications in equipment and electronics, proposed structural uses within European
projects mainly exploited the extreme hightemperature performance of ceramicbased materials for
passive TPS thermal protection systems and thermostructural designs in reusable vehicles, [See:
Chapter70;Chapter71].
The emphasis on ceramics has now changed to dimensionally stable structures, exploiting the low
CTE and electrical characteristics. Although confidence in extreme high temperature performance is
not an issue for such intended applications, lessons learnt in obtaining reliable property data and
analysistechniquesremainappropriate.Likewise,experiencefromotherindustrysectorscanalsobe
applicable.

43.3.1.3

Component design

Thedesignandmanufactureoftechnicalceramiccomponentsissimilartothatofcompositesinthat
they are difficult to machine to final form. Therefore, technical ceramic nearnet shape components
tendtobedesigned,manufacturedandsuppliedbycompanieswiththeexpertise.Althoughtechnical
ceramicscompaniesdoprovidesomestockshapes,themajorityoftheirbusinessisprovidingcustom
components for particular applications. Some general examples include: seals, feedthroughs, wear
componentsinprocessindustries,cuttingtools,heaterelements,rollers,kilnfurniture,heatsinksand
refractoriessuchascruciblesandboats.Thereforemanufacturersandsuppliersoftechnicalceramics
tend to work together with the engineers considering such materials for highperformance
applications.
Good design of ceramic components, as with any other material, aims to exploit the beneficial
characteristicswhilstavoidingthebad,Ref.[4330].

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Thevariousfactorstoconsiderduringcomponentdesigncanbesummarisedas:

Mechanicalloads,[Seealso:43.15designofglassceramics]:

Usecompressiveloadingandavoidtensileorshearloads.

Somematerialsareanisotropic,whereasothersarenot.

Pointloadingisdetrimental,sodistributeloadsasevenlyaspossible.

Physical:

Somematerialsarethermallyconductive,whereasotherarenot.

Thermal expansion is generally much less for ceramics than other materials. In mixed
materialcombinationsthermalexpansionmismatchneedsconsideration.

Someceramicsareelectricallyconductive,othersarenot(insulators).

Some materials become electrically conductive under certain conditions, e.g. high
temperature(zirconia,siliconcarbide).

Shape:

Poorsurfacefinishandfeaturessuchasnotches,sharpcorners,slotsandcutoutsactsas
stressraisersandneedtobeavoidedbyusinggenerousradii.

Largeorsuddenchangesinsectioncanpromotehighthermalstressesandtemperature
gradients.

Joints between ceramics and other materials need careful consideration, e.g. limiting
thermalexpansionmismatchorpointloads.

Holesizes,shapesandpositionneedconsideration.

Nearnet shapes help avoid extensive postmanufacture machining operations that are
difficultorexpensiveandcandamagehard,brittlematerials.

Processing:

The maximum size of highdensity, highperformance materials is generally limited by


theproductionprocessused,e.g.volumeconstraintsofhotisostaticpresschambers.

Processesneedoptimisationtoavoidrepeatedhightemperaturefiringwhichcaninduce
damagebythermalgradientsormismatch.

43.3.2

Property and performance evaluation

43.3.2.1

Test and analysis

Anextensivedevelopmentexercisehasresultedinmethodsofdeterminingthepropertiesoftechnical
ceramicsforengineeringapplications,[See:Testmethods].
Development of models that predict the performance of ceramics (both monolithic and composite)
undervariousconditionsaidsdesignandanalysis.AnexampleistheNASACARESsoftwaresuite,
whichhasbeenappliedtoceramicsdestinedforspaceapplications,Ref.[434].
OriginallyaccesstotheNASAsuiteofsoftwareprogramswasrestrictedtoorganisationswithinthe
USA.Providingthatcertaincriteriaaremet,applicationsfromEuropeanbasedorganisationsarenow
welcomed,Ref.[4349].

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43.3.2.2

NASA CARES software

DevelopedbyNASA,CARESceramicsanalysisandreliabilityevaluationofstructuresisasuiteof
integrated design software tools that provide a means to optimise the design of brittle material
components using probabilistic analysis techniques. It incorporates fundamental mechanics theory
and associated computational approaches for component design using isotropic brittle materials.
CAREScanbegenerallyappliedtodesignsinvolvingtheuseofbrittlematerials(monolithicstructural
ceramics,glasses,intermetallics,andceramicmatrixcomposites)inawiderangeofindustrysectors
and can be used in conjunction with commerciallyavailable FEA packages, e.g. ANSYS and
ABAQUS.
Thesuiteofprogramsincludes,Ref.[434]:

CARESLife, which was developed to predict the reliability and life of structures made from
advancedceramicsandotherbrittlematerials,e.g.glass,carbonsandintermetallics.

CARESCreep, which is an integrated design program for predicting the lifetime of structural
ceramiccomponentssubjectedtomultiaxialcreeploads.Ittakesintoaccountthetimevarying
creepstressdistribution(stressrelaxation).

Composite CARES (C/CARES), which was developed to address aerospace design issues
relating to CMC ceramic matrix composites. The aim is to predict the timeindependent
reliabilityofalaminatedstructuralcomponentsubjectedtomultiaxialloadconditions.

CARES can predict thedurability and lifetime of brittle materials usedforstructuralapplications in


harsh environments, e.g. turbine parts, TPS, radomes, fuel cells and MEMS microelectromechanical
systemsforpowergenerationandpropulsion,Ref.[4350],[4351].
Further developments include enhancement of computational design methodologies for brittle
structures,Ref.[434].

43.3.2.3

Test methods

Traditionally, test methods for technical ceramics were adapted from those used in the refractory,
electricaloropticalindustries,i.e.themainconsumers.Internationalstandardsnowcoveraspectsof
highperformance technical ceramics for engineering applications. These are summarised in Table
43.3.1withdraftstandardslistedinTable43.3.2,Ref.[435],[436].

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Table43.31Technicalceramics:ISOstandardssummary
Number

Date(1)

Title

ISOFineceramics(advancedceramics,advancedtechnicalceramics)(2)
Sample preparation for the determination of particle size
ISO 14703
Mar-2000
distribution of ceramic powders
Test method for flexural strength of monolithic ceramics at
Aug-2000
room temperature
ISO 14704
Jan-2004
ISO 14704 - Technical Corrigendum 1.
Test method for hardness of monolithic ceramics at room
ISO 14705
Mar-2000
temperature.
ISO 15165
Oct-2001
Classification system.
Test method for tensile strength of monolithic ceramics at
ISO 15490
Jul-2000
room temperature.
Test method for fracture toughness of monolithic ceramics
at room temperature by single edge precracked beam
ISO 15732
Oct-2003
(SEPB) method.
Test method for tensile stress-strain behaviour of
ISO 15733
Feb-2001
continuous, fibre-reinforced composites at room
temperature.
Test method for elastic moduli of monolithic ceramics at
ISO 17561
Mar-2002
room temperature by sonic resonance.
Test method for linear thermal expansion of monolithic
ISO 17562
Oct-2001
ceramics by push-rod technique.
Method for flexural strength of monolithic ceramics at
ISO 17565
Dec-2003
elevated temperature.
Determination of absolute density of ceramic powders by
ISO 18753
Aug-2004
pyknometer.
ISO 18754
Aug-2003 Determination of density and apparent porosity.
Determination of thermal diffusivity of monolithic ceramics
ISO 18755
Mar-2005
by laser flash method.
Determination of fracture toughness of monolithic ceramics
ISO 18756
Dec-2003
at room temperature by the surface crack in flexure (SCF)
method.
Determination of specific surface area of ceramic powders by
ISO 18757
Dec-2003
gas adsorption using the BET method.
ISO 20501
Dec-2003
Weibull statistics for strength data.
Determination of adhesion of ceramic coatings by scratch
ISO 20502
Apr-2005
testing.
ISO 20507
Dec-2003
Vocabulary.
Determination of light transmittance of ceramic films with
ISO 20508
Dec-2003
transparent substrate.
Determination of oxidation resistance of non-oxide
ISO 20509
Dec-2003
monolithic ceramics.
Determination of friction and wear characteristics of
ISO 20808
Feb-2004
monolithic ceramics by ball-on-disc method.
Test method for fracture toughness of monolithic ceramics
at room temperature by chevron-notched beam (CNB)
ISO 24370
2005
method.
Key:

(1)Alwaysconfirmwithstandardsorganisationstheversionofastandardiscurrent.

(2)ISOfineceramicsstandardsthatcoverfibrereinforcedcompositesarenotincluded.

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Table43.32Technicalceramics:ISOstandardsdrafts
Number(2)

Date(1)

Title

DraftstandardsFineceramics(advancedceramics,advancedtechnicalceramics)(3)
Test method for air purification performance of
ISO/CD
semiconducting photocatalytic materials -- Part 1:
22197-1
Removal of nitric oxide.
Determination of particle size distribution of ceramic
ISO/CD 24235 powders by laser diffraction method.
ISO/DIS
Determination of thickness of ceramics films by contact18452
probe profilometer.
ISO/DIS
Test method for cyclic bending fatigue of monolithic
Nov-2004
22214
ceramics at room temperature.
ISO/DIS
Test method for tensile creep of monolithic ceramics.
Nov-2004
22215
ISO/DIS
Determination of content of coarse particles in ceramic
Feb-2004
24369
powders by wet sieving method.
Test method for fracture toughness of monolithic
ISO/DIS
Jan-2004
ceramics at room temperature by chevron notched beam
24370
(CNB) method.
ISO/FDIS
Determination of content of coarse particles in ceramic
24369
powders by wet sieving method.
ISO/PRF
Determination of corrosion resistance of monolithic
17092
ceramics in acid and alkaline solutions.
ISO/WD
Determination of tap density of ceramic powders.
23145
Test methods for determination of fracture toughness of
ISO/WD
monolithic ceramics- Single edge V-notch beam (SEVNB)
23146
method.
Key:

(1)Dateincludedforguidanceonly.Alwaysconfirmwithstandardsorganisationstheversionofa
standardiscurrent.

(2)ISOabbreviations:FDIS:Finaldraftinternationalstandard;DIS:Draftinternationalstandard;PRF:
Proofofinternationalstandard;CD:Committeedraft;WD:Workingdocument.

(3)ISOfineceramicsstandardsthatcoverfibrereinforcedcompositesarenotincluded.

43.4

Processing aspects

43.4.1

Manufacturing processes

Owingtothehighmeltingpoint,mosttechnicalceramicmaterialsareproducedbyconsolidatingthe
rawmaterialsintheformofpowders.
Afewofthematerialscanbeproducedbydepositionfromavapourphase.
Ceramicpowdersareavailableinarangeofpurities,particlesizesandsizedistributions,adaptedto
various processing techniques. Additives are used to aid blending (mixing) and as binders to aid
shaperetentioninthegreenformpriortomachiningandfiring.Somepowderstockisblendedwet,
thenspraydriedpriortoprocessingintoagreenshape.

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Various methods of producing shapes have evolved and there can be several variants of the same
basicprocess.Processselectiondependsonsizeandshapeofthecomponentandonproductionrates.
Somemoresophisticatedshapingprocessesincludethedensificationstep.
Figure43.04.1showsaschematicofthepowderprocessingsequence,Ref.[431].

Ceramic powder(s)

Additives
BLEND
SHAPE
(green)
MACHINE
(green)
BAKE
(binder removal)
DENSIFICATION
(firing)
MACHINE
(final)

Figure43.41Technicalceramics:Manufacturingprocesses

43.4.2

Health and safety

Some materials have known toxicological occupational health effects, e.g. beryllia and some man
made vitreous silicate fibres; nanosized materials are also under investigation. Material suppliers
provide material safety sheets that stipulate the necessary handling procedures and protection
measures.
Ceramicprocessinginvolvesworkingwithfinepowdersthatcaneasilybecomedispersed,carriedin
theairandingested.Ingeneral,precautionsarenecessarytocontrolthelevelsofairbornematerials
andalsodebrisresultingfrommachining.
Standardsorganisationsandoccupationalhealthauthoritiesprovideguidanceonthemonitoringand
exposurelevelsforpersonnelworkingwithceramics,Ref.[4341].

43.4.3

Green shapes

43.4.3.1

General

Greenshapesarepartsinanintermediatestatefollowinginitialconsolidationofblendedpowdersbut
priortohighpressureand/ortemperatureprocessesthatgivethedesiredmechanicalproperties.

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Processmethodscanbegroupedbywhethertheblendedpowdersareuseddryorwet.Wetshaping
processesuseavarietyofliquids,suchaswaterorsolvents.These,alongwithvariousadditives,aim
to producean even suspension of ceramic particleswithin a slurry or slip. The liquids areremoved
before firing. Depending on the process, this can involve: evaporation, absorption by the mould
substrate or a drying process applied to the green shape. Common processes for producing green
shapesaresummarisedinTable43.4.1,Ref.[431].

Dry

casting

Slip

SolGel

Extrusion

casting

Tape

moulding

(1)

Wet
Key:

Injection

compaction

Roll

Drypressing

Table43.41Technicalceramics:greenshapeprocesses

(1)Althoughfeedstockiswettoenableinjection,thegreenshapeisdryonejection.

43.4.3.2

Dry pressing

Green shapes are made from dry powders that are placed in a mould and pressed. Variants on the
basictechniqueare:

Uniaxial compaction is a technique that uses a rigid mould and a punch to apply the
compactionpressure.Productionratescanbehighforbothsimpleandcomplexshapes.Using
two punches operating in opposite directions on the same axis with a floating mould aids
compactionandgreencompactremoval.

Wetbag cold isostatic pressing, in which the powder is held in a rubber bag mould and
submerged in a liquid. Consolidation is achieved by pressure transmitted through the liquid.
Thisprocessisfairlyslowandusedforlargeitems.

Drybag cold isostatic pressing, similar to wetbag in that powder in a rubber mould is
pressurised via a liquid, but the rubber mould is integrated into the equipment. This enables
automationandsmallcomponentscanbeproducedathighproductionrates.

43.4.3.3

Roll compaction

Spraydried powders, containing about 5% to 10% of binders and plasticisers, are continuously fed
betweentworotatingrollers.Astherollscometogether,thehighpressurecompactsthepowder.The
tape produced possesses uniform high density and sufficient green strength and flexibility to be
spooled.

43.4.3.4

Injection moulding

A granulated mixture of ceramic and organic binders is charged into the machine and the air
removed. A heated charge is then injected into a cold die cavity, where it cools slightly prior to
ejection.
Usuallyformakingsmall,complexshapedgreencomponents,injectionmouldinghasalsobeenused
forprototypingcomplexengineparts,suchasrotorsandturbinesinturbochargers.

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43.4.3.5

Tape casting

Tape casting is based on the patented Park process and is also known as doctor blade or knife
casting.
A slurry or slip is produced from a suspension of ceramic powder in a liquid along with additives
appropriatetothematerialsanddensificationprocess,e.g.binders,plasticisersanddeflocculants.The
slipisthenfedontoapolymersheetthatpassesunderablade.Theheightofthebladecontrolsthe
thickness of the ascast sheet or tape. After drying, to remove the solvent, the green tape is then
spooled.
Theprocessisusedformakingcontinuousthinsheetsortapesofceramic,oftenusedassubstratesfor
electronicdevices.

43.4.3.6

Extrusion

Aslurryisproducedfromceramicpowdermixedwithwater,anorganicsolventorsometimespitch.
A variety of additives are used to adjust the flow characteristics of the mix and to ensure sufficient
greenstrengthafterextrusion.
The slurry is then forced through the extrusion die to form continuous green compacts of constant
crosssection,e.g.tube,rod,channelandhoneycombsections.

43.4.3.7

Sol-Gel

The Sol is a liquid colloidal solution containing dissolved metallic salts or organic compounds. A
rigid Gel is formed from the solution and is then dried prior to densification (firing). The basic
technique has many variables, enabling a wide range of compositions and products, including:
shapes,films,fibresandverylowdensity,porous,aerogels
The process is used for exceptionally fine, pure ceramics, e.g. ultra fine grained alumina and some
specialitycompositionsforfunctionalelectronicdevices.
Owingtothereactivenatureoftheceramicproduced,thesinteringtemperaturesarelowerthanthose
necessaryforconventionallyproducedmaterials.
SolGels are also used in the manufacture of ceramic matrix composites, where the Sol is infiltrated
intoafibrepreformwhichactsasadepositionsubstrate,[Seealso:88.16].

43.4.3.8

Slip casting

Slip (or slurry) is a liquid suspension of ceramic particles, usually in water, containing various
additives to aid processing. This is poured into or over a porous mould (usually plaster), which
absorbs some of the water near the interface. Excess liquid slip is then removed leaving the green
shapeincontactwiththemould.Themouldedthicknesscanbecontrolledbyprocessparameterssuch
astheliquidcontentofthesliportimeincontactwiththemould.Thegreenshapeisremovedfrom
themouldanddriedpriortofiring.
Slip casting is a widelyused traditional processing technique within the ceramics industry. It can
producelarge,complexshapeditems.

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43.4.4

Densification

43.4.4.1

General

Following a drying process, the majority of green shapes are densified by sintering (firing).
Dependingonthematerialcompositionandtemperature,thedensificationprocessisdifferent.

43.4.4.2

Liquid-phase sintering

At the sintering temperature a small quantity of liquid phase forms, less than needed to fill all the
voids. The remaining solid phase is soluble in the liquid and fills the voids by a combination of
diffusion,dissolutionandredeposition.

43.4.4.3

Viscous-flow sintering

Part of the material melts at the sintering temperature and flows by capillary action into the voids.
Aftercooling,thisphasecanbecrystallineorglassy.

43.4.4.4

Solid-state sintering

During sintering no liquid phase forms and consolidation is by solidstate diffusion only. Fine
powdersandhightemperaturesarenecessaryforthisprocess.

43.4.4.5

Reaction bonding

Mixtures of suitable ceramic powders are subjected to conditions that enable a chemical reaction
between the constituents, forming a densified product, e.g. high temperatures and reactive gaseous
atmospheres.Reactionscanoccurinthesolid,liquidorgaseousstates.
Siliconcarbideandaluminiumnitridecanbothbeproducedbythesemethods,e.g.C+SiSiC;2Al+
N22AlN.

43.4.5

Combined shaping and densification

43.4.5.1

Hot pressing

Powders are enclosed in a die, often made from graphite to enable induction heating. Heat and
pressurearethenapplied.Dependingonthematerialcompositionandtemperature,densificationcan
beliquidphaseorsolidstate.
Hotpressingislimitedtofairlysimpleshapes.Machiningofdensifiedshapesneedsveryhardtools.

43.4.5.2

HIP - hot isostatic pressing

TheceramicpowdersaresealedintoametalorglasscapsuleandthenloadedintotheHIPpressure
vessel. Highpressure gas, usually argon, compacts the powder at high temperature. The sintering
processcanbeliquidphaseorsolidstate.Theconsolidatedmaterialscanapproachfulltheoretical(i.e.
voidless)density.
HIP is also used as a final or remedial process to close voids and increase the density of materials
processedbyothertechniques.
Complex shapes can be consolidated effectively by HIP, but the capacity of the HIP pressure vessel
limitsthesizeofcomponents.Machiningofthedensifiedshapeneedsveryhardtools.

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43.4.6

Vapour-phase techniques

43.4.6.1

General

There are several processes in which ceramic materials are deposited from a chemical atmosphere
ontoasubstrateathightemperatures.Thesizeandshapeofcomponentsproducedarelimitedbythe
processvesseldimensions.
Vapourphase processes are also used for the manufacture of ceramic matrix composites, where the
fibrepreformactsasthedepositionsubstrate,[Seealso:Chapter88].

43.4.6.2

Chemical vapour deposition

Thedecompositionofagasmixturecontainedinapressurevesselathightemperaturedepositshigh
puritymaterialontoasubstratesurface.Materialpropertiestendtobeanisotropic.
CVDisnormallyusedtocreatethinwalledshapesorcoatings.Processtimesareusuallyquitelong,
but can be decreased by a modified technique using a plasma around the substrate; known as
PACVD, plasmaassisted CVD. CVI chemical vapour infiltration is a CVD technique in which the
materialisdepositedonandbetweenthefibresofapreformtocreateaceramicmatrixcomposite.
CVDisusedtoproducesyntheticdiamondmaterialsandshapesforavarietyofwearparts,thermal
managementandopticaluses,Ref.[438];[Seealso:43.17].

43.4.6.3

Physical vapour deposition

One or more materials transform from the solid state into a vapour phase under vacuum and then
condenses onto a substrate. PAPDV, plasmaassisted PVD, enables virtually any material to be
depositedasacoatingontoanonporoussubstrate.

43.4.7

Machining

Althoughcomprisingofcompactedabrasivepowders,thestrengthofgreenshapes(greenstrength)is
sufficient to enable them to be machined fairly easily without the need for expensive, hard cutting
tools. The majority of features tend to be moulded into the shape rather than machined. Where
necessary, machining is used in the green stage to reduce as far as possible the need to machine
componentsafterfiring.
Densified materials are much more difficult to machine due to their hard, brittle nature. Machining
operationsareusuallylimitedtofinishingsurfacesusingveryhardgrindingmedia.

43.4.8

Joining

43.4.8.1

General

Techniquesforjoiningceramicscanbeclassedasthoseusedtoassemblegreenshapes,priortofiring,
orthoseusedtoassemblefullydensifiedmaterials(postfiring).
Somerecentnoveltechniquesinvolvediffusionbonding,theuseofcompatibleinterlayersandlocal
infiltration to produce joints. Processes using microwave heating and ultrasonics are also under
developmentforceramics,Ref.[4348].

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43.4.8.2

Green shape assembly

Largeitems,oftenofcomplexshape,canbeproducedasaseriesofsubcomponentswhicharethen
joinedpriortofiring.Dependingonthematerialandtheprocesstechniqueusedtocreatethegreen
part,aslipofthesame,oracompatiblematerial,canbeusedasadhesive.Afterbakingtoremove
moistureorsolvent,thepartisfiredandtheslipformsabond.
Some ceramicbased adhesives can be used instead of slip provided that their firing temperature is
compatiblewiththecomponentdensificationtemperature.

43.4.8.3

Fully-densified materials

The choice of assembly method largely depends on the application and service environment. The
main problems to consider are avoiding point or uneven loads and thermal mismatch between the
ceramicandadjacentparts;bothofwhichcancausefractureinceramics,Ref.[4348].
Ceramic parts can beretained withinmetal components byshrinkfitting. Thisrelies on the thermal
expansion differences between metals and ceramics to produce a compressiontype joint when the
mixedmaterial component has cooled. This process is widelyused for locally increasing the wear
resistance ofengineeringparts,suchas thread guides in process machineryand for the assembly of
sparkplugs.
Mechanical fastening can be used providing that point and uneven loads are avoided. Mechanical
seals are used to position and retain ceramic parts between other materials, e.g. Oring seals to
positionequipmentwindows.
Bondedjointsarelimitedbytheworkingtemperaturerangeoftheadhesive.Ceramicbasedadhesives
can be used for bonded assemblies in hightemperature applications. These adhesives usually need
firing,butthiscanbeatalowertemperaturethanthedensificationprocess.Conventionaladhesives
canalsobeusedprovidingthattheytoleratethethermalconditions,adheretothesurfacesandhave
sufficientmechanicalperformance.
Some ceramics are assembled by brazing, where the metalbased filler is used as the adhesive, e.g.
assemblyofceramictipsandinsertsontometaltoolsupports.Toensurethequalityofbrazedjoints,
the surfaces of ceramic parts are metallised with a thin metalrich coating in order to improve
adhesion with the braze filler. Thermal gradients created during brazing need to be minimised to
avoid possible failures. To limit thermal gradients, assemblies are often heated prior to brazing and
cooledslowlyandevenlyafterwards.

43.5

Applications

43.5.1

Industrial

Technical ceramics have proven success in many diverse applications covering a wide range of
industry sectors, e.g. from aggressive environments in the petrochemical process industries to
prostheticbiomedicalimplants.

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43.5.2

Aerospace

43.5.2.1

General

Withintheaerospaceindustryasawholemonolithictechnicalceramicsarewidelyusedinequipment
andpayloads.Someapplicationsarebasedsolelyonelectricaloropticalperformance,e.g.electrical
electronic components and assemblies, sensors or optics; whereas others are, to some extent, load
bearing.Theseareoftenstaticloadsbutareincreasinglybeingusedindynamicsituations,e.g.pump
parts,suchasbearings,valvesorseals;withincombustionchambers;turbochargers;discsinbraking
systems.
Ceramicsarenowusedforthemirrorsandstructuresofscientificspaceinstrumentsthatneedhigh
stiffnessandstability.Ceramicsalsoofferinterestingpropertiesforcryogenicapplications.

43.5.2.2

Environment components

Technicalceramicsareselectedtoresisttheworkingenvironmentthroughouttheservicetemperature
range for the intended service life. Depending on the aerospace application, the environment for
technical ceramic engineering components can range from high to low temperatures, and include
contactwithgases,fluidsorsolids,e.g.nozzles,pumpparts,seals.

43.5.2.3

Environment structures

Forstructuralapplications,theenvironmentscomprise:

Earth, during manufacture and storage. Ceramics are rarely 100% densified, so retain some
level of residual porosity. If not properly controlled, moisture and contaminant uptake is
possible unless exposed surfaces are sealed. Sealing is an established process for technical
ceramics in direct exposure to chemical environments. A bakeout process is often used to
removecontaminantsbeforeoraftersealing.

Launch; where conditions are largey dictated by the launch vehicle, e.g. vibration levels. For
ceramictype materials, the effects of dynamic loads need evaluation as do any interfaces
betweentheceramicsandadjacentmaterials.

Spaceenvironment(missionrelated).

43.5.2.4

Environment space

Although levels are missiondependent, the general effects of the space environment on technical
ceramicsaresummarisedas,[Seealso:ECSSQ7071]:

Vacuum: provokes outgassing of residual, processrelated, materials and moisture.


Componentstobeexposedtovacuumareusuallybakedoutandsealed(glazed).

Radiation:levelsinspacehavenoknowneffectsonthecharacteristicsofceramics.

Temperature:Hightemperatureperformanceisamainreasonforselectingceramics.However,
the upper working temperature varies for different groups of materials, especially when
combinedwithanaggressivechemicalenvironment,e.g.carbonbasedmaterialsinoxygenrich
environments.

Thermalcycling:cancausecrackinginceramicsduetoshapeeffectsandthermalgradients.

Atomicoxygen:hasnoknowneffectonceramics.

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43.5.3

Materials

43.5.3.1

General

Whilst some materials are used for many different applications, others tend to be more limited to
exploitaparticularcharacteristic,e.g.IR,microwaveorradartransparency.
Excludingtheabrasiveandcuttingtoolssector,manufacturersandstandardsorganisationsalike,tend
togrouptechnicalceramicsbytheirusualtypeofapplications,Ref.[435],e.g.:

mechanicalcomponents,

thermomechanicalcomponents,

chemical components, include items used in industrial processing which are often in very
aggressive environments (acids, alkalis, chemical slurries, liquid metals, abrasive). Corrosion,
oftenathightemperatures,orwearresistancearethemainselectionfactors.

electricalinsulators,asdefinedinIEC672EN606721,Ref.[437].

electricalconductors,usedinfuelcells,batteries,heatingelements,gassensorsandelectrodes;
staticdischarge.

functional electrical materials, which exhibit dielectric properties or characteristics, e.g.


ferroelectric,piezoorpyroeffects.

magneticmaterials.

Whilstalloftheseapplicationsexisttosomeextentwithintheaerospaceindustry,onlythosewhich
usually provide some degree of loadbearing capability combined with the specialist properties of
ceramicsarepresentedhere.Materialsconsideredfordimensionallystableandopticalstructuresare
alsoincluded.

43.5.3.2

Mechanical components

Some technical ceramics commonly used for discrete, often simplyshaped, mechanical components
are summarised in Table 43.5.1. These items usually provide a level of loadbearing combined with
wearorcorrosionresistance.

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Bearings*

Injectorpins(fuel)
Pumps*

(1)

Seals*(shaft)

(1)

Seals*(mechanical)

(1)

Valves(ball)

Valves(pneumatic)

Valves(trains)
Key:

Glassceramics

Zirconia

(1)

Bearings(ballroller)
Bearings(sleeve)

Siliconnitride

Siliconcarbide

Silicas

Diamond(CVD)

Carbons

Boronnitride

Boroncarbide

Aluminas

Aluminiumnitride

Table43.51Technicalceramics:Materialsmechanicalcomponents

*wearresistance;primarymaterial;secondarymaterial;(1)carbongraphites

43.5.3.3

Thermomechanical components

Technical ceramics for hightemperature technologies are summarised in Table 43.5.2. These can be
relativelylarge,complexshapeditemsoperatingathightemperaturesinhostileenvironmentsunder
dynamic or static load conditions. Carboncarbon and ceramic matrix composites have also been
evaluatedforsomeoftheseapplications,[See:SectionXII].

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Table43.52Technicalceramics:Materialsthermomechanicalcomponents

Combustionchambers
(diesel)

(1)

Jetengine(combustors)

Jetengine(petals)
Rocketnozzles

(1)

Turbocharger(housings)

Turbocharger(rotors)

Valves(reciprocating
engines)

Key:

TPS(active)
TPS(passive)

CMC(3)

CarbonCarbon(2)

Glassceramics

Zirconia

Siliconnitride

Brakediscs

Gasturbines

Siliconcarbide

Silicas

Diamond(CVD)

Carbons

Boronnitride

Boroncarbide

Aluminiumnitride

Aluminas

TPSthermalprotectionsystem;primarymaterial;secondarymaterial;
(1)carbongraphites;(2)[See:Chapter54];(3)[See:Chapter52]

43.5.3.4

Electrical

Theprimarycriterioninselectingtechnicalceramicsforelectricalandelectronicusesistheinsulating
or electrical conductivity behaviour. Service temperature can affect this, e.g. zirconia becomes
conductiveathightemperatures.
Table43.5.3summarisessomeofthosetechnicalceramicswhichareusedasinsulatorsorconductors.
Onlyafewexamplesareprovidedforelectricalandelectronicapplicationsfromthosethatconstitute
alargeproportionofthetechnicalceramicmarket.

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Table43.53Technicalceramics:Materialselectrical

INSULATORS(1)
Electronicdevices

(3)

Glassceramics

(2)

Electrodes

Heatingelements
Key:

Zirconia

CONDUCTORS

Fuelcells

Machinable

Batteries

(2)

(3)

Highstrength

Radomes

Siliconnitride

Siliconcarbide

Silicas

Diamond(CVD)

Carbons

Boronnitride

Boroncarbide

Aluminiumnitride

Aluminas

(1)Foracomprehensivelistofinsulators,See:IEC672EN606721:Definitionsandclassifications;
(2)Zirconiaisconductiveathightemperatures;
(3)highthermalconductivity;
primarymaterial;secondarymaterial

43.5.3.5

Dimensionally-stable and optical structures

Technicalceramicsforopticalapplicationscanbegroupedas:

optical devices and components, which are transparent to particular wave lengths, e.g.
windows,lasercomponents.

mirrors and support structures for optical systems; providing highly stabilty and minimising
thermal expansion problems which can affect system performance, e.g. telescopes, mirrors,
antennas.

Excluding glasses, Table 43.5.4 gives examples of technical ceramics that are considered for some
opticalapplications,[Seealso:Casestudies43.18;43.19].

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Table43.54Technicalceramics:Materialsopticalanddimensionallystable
structures

Lasercomponents

(1)

(2)

Mirrors(Xray)

Optical(support
structures)

Telescopes
(1)

Glassceramics

Zirconia

Mirrors

Windows(visible

andinfrared)

Siliconnitride

Siliconcarbide

Silicas

Diamond(CVD)

Carbons

Boronnitride

Boroncarbide

Aluminiumnitride

Aluminas

Key:primarymaterial;secondarymaterial;(1)rubyorsapphire;(2)mirrorsfortelescopes

43.6

Aluminium oxide: Alumina

43.6.1

Typical characteristics

43.6.1.1

Standard grades

Commerciallyavailablealuminamaterialsaregenerallygroupedby:

Form,e.g.powders,granulesorpellets,shapesorcomponents.

PurityandcompositionusuallystatedasthepercentageoftheAl2O3content.Somegradesalso
giveacompositionifanadditionofanothermaterialisincluded,e.g.alumina+zirconia.Trace
elements,orimpurities,arerarelystated.

Crystalsize,inthemicronrange.

The majority of engineering grades are opaque white, although pinks and browns also exist. Some
gradesaretranslucent,[See:Specialgrades].
Thepurityandcrystalsizeaffectthepropertiesofthedensifiedmaterials.

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Basicfeaturesofaluminamaterialsinclude:

Mechanical: high stiffness, hard and brittle; toughness and strength improved by Zirconia
additions(ZTAgrades).

Thermomechanical:propertiesaregenerallyretainedtoabout800C,butreducesignificantly
above1000C;mediumshockandthermalcyclingresistance.

Electrical:nonconductive;excellentelectricalinsulation.

Environment:chemicalresistancetobothacidandalkalis(exceptHF).

43.6.1.2

ZTA Zirconia toughened alumina

ZTAishigherinstrengthandtoughnessthanconventionalaluminagrades.Thisresultfromastress
inducedtransformationtougheningeffectachievedbyincorporatingabout10%to20%finezirconia
particlesuniformlythroughoutthealumina.

Typicalcharacteristicsinclude:

Strength,

Toughness,

Wearresistance,

Hightemperaturestability,

Corrosionresistance.

ZTAgradesareusedinmechanicalapplications,suchaswearparts,valveseats,pumpcomponents,
bearings,bushes.

43.6.1.3

Special grades

Translucentaluminaisusedforhighertemperature,opticaluses,suchaslighting.
Syntheticsapphireisasinglecrystalformofalumina,whichisusedinopticalapplications,e.g.laser
systemsandwindowsforimagingsystems[Seealso:43.16].

43.6.2

Typical properties

43.6.2.1

General

The properties stated by manufacturers of alumina materials depend on the form in which the
materials are supplied and also their main applications. It is unusual to have a complete set of
mechanical,thermomechanical,physicalandelectricalpropertiesforanyparticulargradeofmaterial.

43.6.2.2

Powders

Powderpropertiesoftenstateanaveragepowdersize,althoughsomegiveparticlesizedistributions.
Density values can be for loose powder, tamped or green state (compacted but not fired). Some
suppliersgiveanindicativebulkdensityforadensified(fired)material.

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43.6.2.3

Shapes and components

Density values are given along with a typical porosity level, which can be stated as % apparent or
open(interconnectingpores)or%closedandinterconnectingpores.
For some applications, porous alumina grades are needed, e.g. thermal insulation and catalytic
supports.
Commonlystatedmechanicalpropertiesaresomecombinationof:

Hardness(onvariousscales),

Compressiveproperties(strengthandmodulus),

Flexuralstrength,

Fracturetoughness.

Tensilepropertiesarelesscommonbecausesuppliersassumethatapplicationsavoidusingceramics
undertensileorbendingloads.
Thermalcharacteristicsoftenstatedareacoefficientofthermalexpansion,thermalconductivityanda
maximumusetemperature,usuallyinair.Somealsoprovideathermalshockvalue.
Electrical characteristics stated can include dielectric properties and volume resistivity at various
temperatures.
Table43.6.1summarisesthepropertiesofsomeexamplesofdensifiedcommercialaluminamaterials,
[4312].
The grades presented, taken from a much wider range of alumina products, are all used in load
bearing,mechanicalapplicationsratherthanforelectricalorthermalcharacteristicsalone.
The large number of grades available has evolved over the years to meet particular applications in
various industry sectors. In general, this is to achieve a balance between the wear, chemical,
mechanicalandothercharacteristics.Gradeshavealsobeendevelopedforspecialistapplications,e.g.
ballisticprotection.
Althoughthematerialscitedallcomefromonesource,italsoillustratestherangeofmaterialsthatare
availablefromothermajortechnicalceramicssuppliers.

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Table43.61Technicalceramics:aluminatypicalproperties

HILOX 961
MAC-A960S

HILOX 882
MAC-A840S

SINTOX FL
MAC-A950R-6

SINTOX FF
MAC-A950R-5

SINTOX FC
MAC-A950R-4

SINTOX AL
MAC-A997R

DERANOX 975
MAC-A975R

95

96

95

99.7

97.5

2.8

3900

3790

3880

3530

3720

3700

3720

3200

3800

0
86

0
83

0
84

0
76.4

0
14.6
-

0 (4)
12.5
78

0
14.6

20(3)
-

0
15
85

2100

1800

2500

2000

2500

2500

370

283

376

271

325

320

325

150

350

336

354

250

330

325

330

340

5.9

4.5 (2)

5.9

3.6

21

15

20

21

20

24

8.2

8.2

8.2

7.5

7.5

7.5

9.0

8.1

Wear parts, pumps, shafts, bearings,


seats; valve seats; pneumatic valve
sliders

Wear parts, pumps,


shafts, bearings, seats

Automotive water pump parts

Dynamic pump parts for


corrosive media; wear parts

Aerospace parts (non outgassing);

Dynamic pump parts for corrosive


media; wear parts

Laser reflectors

Dynamic and static components; pumps,


valves; chemical or abrasive
environment

Alumina content (%,


typical)
Grain size (m)
Bulk density (fired)
(kg/m3)
Porosity apparent (5) (%)
Vickers (GPa, Hv0.5kg)
Rockwell (R45N)
Compressive strength
(MPa)
Flexural strength (1)
(MPa)
Youngs modulus (GPa)
Fracture toughness
(MPa m1/2)
Thermal conductivity
(WmK, 20C)
Coefficient of thermal
expansion, 20C to
1000C (10-6 /C)

Applications(examples)

99

HILOX 965
MAC-A955S

84

HILOX 991
MAC-A990S

Property

Key:

96

95 96
-

Wear parts, pumps, shafts, bearings,


seats (chemical environment)

Examplesofcommerciallyavailablealuminagrades

SINTOX,HYLOXandDERANOXaretrademarksofMorganAdvancedCeramics.(1)
3pointbend(ASTMC1161),20C;(2)K1C(SENB);(3)Porousgradeforlaser
reflectors;pumpingchambers;(4)Nonoutgassingforaerospaceapplications;
(5)Fullydense.

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43.6.2.4

ZTA Zirconia toughened alumina

Table 43.6.2 summarises properties of an example of a ZTA commerciallyavailable material


comparedwithanaluminagradeusedforsimilarmechanicalapplications,Ref.[4312],[4332].

Table43.62Technicalceramics:ZTAzirconiatoughenedaluminatypical
properties

Property
Composition
Zirconia content (%, typical)
Grain size (m)
Bulk density (fired) (kg/m3)
Porosity apparent (%)
Hardness, Knoop (GPa, 1000g)
Rockwell (R45N)
Compressive strength (MPa)
Flexural strength (1) (MPa)
Flexural strength (2) (MOR, MPa)
Youngs modulus (GPa)
Fracture toughness (MPa m1/2)
Thermal conductivity
(WmK, 20C)
Coefficient of thermal expansion, 20C
to 1000C (10-6 /C)
Key:

Comparisonofcommerciallyavailablegradesof
aluminawithZTA
ZTA
HILOX 965
Zirconia-toughened
Alumina
alumina
0
not stated
2
3790
4050
0
14.4
83
85
2900
450
283
336
360
5 to 6
-

27

8.2

8.3

ZTACoorsTekproduct;HILOXisatradenameofMorganAdvancedCeramics;(1)3
pointbend(ASTMC1161),20C;(2)ASTMF417

43.7

Aluminium nitride

43.7.1

Typical characteristics

Generalfeaturesofaluminiumnitrideceramicsinclude:

highthermalconductivity

goodelectricalinsulation.

Thethermalandelectricalpropertiesdependonpurity.Powderformsarepronetomoistureuptake
that can affect electrical properties. Some typical applications include uses in the semiconductor
processingindustry,heatmanagementinelectronicsandwindowsforvisibletoinfraredsystems.

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43.7.2

Typical properties

43.7.2.1

General

Table 43.7.1 summarises properties for some examples of commerciallyavailable aluminium nitride
materials,Ref.[4314],[4315].

43.7.2.2

Shapal machinable grade

ShapalisproducedbyTokuyama,JapanbutisavailableinEuropefromdistributors.TheShapal
grades are highpurity, machinable aluminium nitrides, which offer strength and thermal
conductivity.ShapalMisamachinablegradeandShapalSH15istranslucenttovisibleandIR
light.
Thethermalconductivityisnotashighasstandardaluminiumnitride,butisabout50timesgreater
thanthatofmachinableglassceramics,[Seealso:43.15]
TheabilitytomachineShapalwithconventionalcarbidetoolsmeansthatmorecomplexshapescan
bemadecomparedwithstandardaluminiumnitrideceramics.
Applications are similar to standard grades, e.g. substrates for semiconductors; heat sinks and
insulating parts for highpower electronics; window materials for infrared and radar applications;
refractories(moltenmetals).

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Table43.71Technicalceramics:Aluminiumnitridetypicalproperties

Key:

3300

3260

1110

1000

1100

200
320

200
320

3.0

330
320

340
0
10.
8
290
320

340
0
10.
4
310
320

340
0
10.
4
310
320

220
310

3.0

2.5

170

170

80

150

160

150

67

6.2

5.6

4.9

AN 2000

AN 216A

3300

AN 217

99.8
4

AN 215

CERALLOY
13701E

99.0
10

99.9 (2)
3200
-

5.4

5.4(

5.3(

(1)

1)

1)

5.2(1)

Semiconductor devices (IC packages)

Semiconductor devices (IC packages)

Semiconductor processing industry;


Plates for uniform heating; High
temperature supports

11.2

Semiconductor devices (IC packages)

Hot pressed; Semiconductor components;


Gas distribution

Applications(examples)

CERALLOY
1370CS

Rockwell (R45N)
Compressive strength (MPa)
Flexural strength (MPa)
Youngs modulus (GPa)
Fracture toughness (MPa
m1/2)
Thermal conductivity
(WmK, 20C)
Coefficient of thermal
expansion, 20C to 1000C
(10-6/C)

98.0
10

Hot pressed; Semiconductor components

AlN content (%, typical)


Grain size (m)
Bulk density (fired) (103
kg/m3)
Porosity apparent (%)
Hardness (kg/mm2)
Vickers (GPa, Hv0.5kg)

Sintered; Semiconductor components;


microwave parts

Property

CERALLOY
1370DP

Examplesofcommerciallyavailable
aluminiumnitridegrades

CERALLOYisatradenameofCeradyneInc.,ANgradesarefromKyoceraCorp.;(1)
CTE40Cto800C;(2)Highpuritygrade.

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43.8

Boron carbide

43.8.1

Typical characteristics

Boroncarbidehasalowdensity(2500kg/m3)andahardnessapproachingthatofdiamond.
Generalfeaturesofdensifiedboroncarbideinclude:

Lowdensity.

Highmodulus.

Extremelyhard.

Susceptibletothermalshock.

Excludingabrasives,typicalapplicationsareforwearresistance,e.g.nozzles(processingequipment),
dies, precision engineering parts. It also has some specialist applications such as impact resistance
(ballisticarmour)andinnuclearshielding(neutronabsorption).
Boroncarbidecanbeprocessedinapowderformorproducedbyvapourphasetechniques.

43.8.2

Typical properties

Table 43.8.1 summarises the properties of some examples of commerciallyavailable boron carbide
materials,Ref.[4314].

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Table43.81Technicalceramics:boroncarbidetypicalproperties

Key:

CERALLOY
546-3E (1)

CERALLOY
546-4E

98.5
15

99.5
15

2500

2500

2500

3200
410
460

2800
410
460

3200
410
460

2.5

2.5

2.5

90

90

90

5.6

5.6

5.6
Hot pressed; ballistic armour;
semiconductor processing; wear
parts.

Applications(examples)

98.5
15

Hot pressed; semiconductor


processing.

B4C content (%, typical)


Grain size (m)
Bulk density (fired) (103
kg/m3)
Porosity apparent (%)
Hardness (kg/mm2)
Vickers (GPa, Hv0.5kg)
Rockwell (R45N)
Compressive strength (MPa)
Flexural strength (MPa)
Youngs modulus (GPa)
Fracture toughness (MPa
m1/2)
Thermal conductivity
(WmK, 20C)
Coefficient of thermal
expansion, 20C to 1000C
(10-6 /C)

CERALLOY
546

Property

Hot pressed; ballistic armour;


semiconductor processing; wear
parts.

Examplesofcommerciallyavailableboron
carbidegrades

CERALLOYisatradenameofCeradyneInc.;(1)Highpurity,singlephase,lowporosity
grade.

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43.9

Boron nitride

43.9.1

Typical characteristics

43.9.1.1

General

Boronnitrideiscommerciallyavailableas:

Hexagonal boron nitride. (H-BN);

Cubic boron nitride (C-BN).

Pyrolytic boron nitride (PBN), produced by a vapour-phase process.

ThecharacteristicsofHBNandCBN,dictatedbytheircrystalstructures,aretotallydifferent.

43.9.1.2

H-BN - hexagonal boron nitride

HBN has a graphitelike crystal structure. The lattice layers and platelike structure provide good
lubricatingproperties.HBNisusuallyformedbyhotpressingbecauseofitsresistancetosintering.
FeaturesofHBNinclude:

Hotpressedblankscanbemachined,usingconventionaltechniques,tomakecomplexshaped
parts,

Anisotropicproperties,whenproducedbyhotpressing,

Goodelectricalproperties(dielectricstrength;resistivity).

Highchemicalresistance(resistanttomostmoltenmetals,glasses,salts),

Excellentlubricatingproperties,

Excludinglubricants,HBNisusedforshapedpartsinmaterialsprocessingindustries,includingHIP
produced ceramics, due to its nonwetting capability; hightemperature electrical insulators (about
850Cinairduetoitstendencytooxidise;about1350Cininertorreducingatmospheres).

43.9.1.3

C-BN - cubic boron nitride

ThestructureofCBNisthesameasdiamondanditscharacteristicsareverysimilar.Generalfeatures
ofCBNinclude:

Hardnessapproachingthatofdiamond,

Excellentwearresistance,

Highthermalconductivity,

Goodchemicalinertness.

Excludingabrasives,CBNisusedforcuttingtools,wearresistantparts,coatingsandsubstratesfor
highpowerelectronicdevices.

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43.9.1.4

PBN - pyrolytic boron nitride

PBNisahighpurity,pyrolyticmaterialformedbyavapourdepositionprocess.Thestructureofthe
depositedPBNishexagonal,asshowninFigure43.9.1,Ref.[4317].

Figure43.91Technicalceramics:pyroliticboronnitridestructure
AswithHBN,PBNishighlyanisotropicinitselectricalandmechanicalproperties,butveryresistant
tothermalshock.Itisalsoaverygoodelectricalinsulatorandhasveryhighthermalconductivity.The
material is stable in inert and reducing atmospheres up to 2800C, but only to 850C in oxidising
atmospheres.
Itsgeneralfeaturesinclude,Ref.[4312]:

Lowdensity,

Highthermalconductivity,

Lowthermalexpansion,

Goodthermalshockresistance,

Highelectricalresistance,

Lowdielectricconstantandlosstangent,

Goodchemicalresistance.

PBN is used for thinwalled electrical insulators, heating element parts and components for the
semiconductorprocessingindustry.

43.9.2

Typical properties

Table 43.9.1 summarises properties for some examples of commerciallyavailable boron nitride
materials,Ref.[4312],[4316],[4317].

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43.9.3

Space application examples

43.9.3.1

Combat boron nitride grades

Several of the St. Gobain (formerly Carborundum Corp.) Combat boron nitride grades have been
usedininsertsinHalleffectthrusters,Ref.[4316].
Hall effect thrusters were invented in the USA and developed into the SPT stationary plasma
thrusterintheexUSSR.Thethrustersaresmallrocketenginesthatuseapowerfulmagneticfieldto
acceleratealowdensityplasmaandsoproducethrust.
CombatgradesMandM26,alongwithHPandAX05,havebeenfabricatedintoawidevarietyof
thrusterinserts.Eachgradehasdemonstratedsputtererosionresistance,secondaryionemission,gas
absorptionandoutgassingthatarewellwithinthenecessarylimits,Ref.[4316].

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Table43.91Technicalceramics:boronnitridetypicalproperties

COMBAT
AX05 Grade

COMBAT
ZSBN Grade

COMBAT
M Grade
(40%BN + 60%
Silica)

HBR Grade
(calcium borate)

40
-

94
-

1920

1900

1910

2000

2.9
19.9
-

15.3
16.4
-

14.2
4.2
-

100
1.4
-

11
-

218
5
-

Compressive strength (MPa)

143.3

30.1

17.9

31.7

68.9

255

23.4
17.9
21.4

36.8
106.9
144.1

44.5
43.7
60.2

62.0
51.7
41.3

331

Flexural strength (MPa

186.6
75.8
113.0

70.8

62.0

70.5

48.2

23.
4
-

19.4
33.7

27.0
29.0

78.0
130.0

22.6
40.2

55
33

11.85

2.95

1.0

3.2

0.87

0.3

Electrical insulators; high-purity


materials processing; Vacuum parts;

Electrical insulators; High-purity


materials processing (shapes, crucibles).

Youngs modulus (GPa)


Fracture toughness (MPa
m1/2)
Thermal conductivity
(WmK, 20C)
Coefficient of thermal
expansion, (10-6 /C) 20C to
1500C

Applications(examples)

Key:

PBN

COMBAT
HP Grade
-

Electrical insulators; high-purity


materials processing; Thermo-electrical
(radar parts, antenna windows); Thruster
inserts
Electrical insulators; high-purity
materials processing; Thermo-electrical
(radar parts, antenna windows); Thruster
inserts
High-temperature mechanical
components (fixtures, jigs, bearings,
valves)
Thermoelectrical; thermomechanical
(materials processing, thermal shock and, chemical resistance); Thruster
inserts

COMBAT
A Grade
-

BN content (%, typical)


Grain size (m)
Bulk density (fired) (103
kg/m3)
Porosity (%)
Hardness Knoop (kg/mm2) (1)
Vickers (GPa, Hv0.5kg)
Rockwell (R45N)

Electrical insulators; high-purity


materials processing; Thermo-electrical
(radar parts, antenna windows)

Property

Direction (2)

Examplesofcommerciallyavailableboronnitridegrades

193

COMBATisatradenameofSaintGobain,HBRisatradenameofGEAdvancedCeramics;
(1)averagevalues;(2)Pressingorcrystaldirection;(3)OtherGEAdvancedCeramicgrades
available,includingcompositemixtureBN+AlNgrade;PBNdatafromMorgan
PerformanceMaterials.

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43.9.3.2

Sintec Keramic boron nitride grades

Boron nitride grades from Sintec Keramic (D), have been used in the propulsion system on the
SMART1spaceprobe,Ref.[4345]:

BNcomposite,usedintheplasmachamber.

PBNparts,usedintheelectricalfeedofthePPSthruster.

LaunchedSeptember2003,SMART1wasthefirstESAspaceprobetogototheMoon.Itsaimswere
totesttheadvancedtechnologyneededforfuturescientificplanetarymissions.Thisinvolvedtesting
miniaturisationtechnologywhilstexploringtheMoonfromorbit,Ref.[4346].

43.10

Carbon

43.10.1 Typical characteristics


43.10.1.1 General
Carbonmaterialsareavailableinavarietyofformswithwidelydifferingcharacteristics,e.g.:

Graphite, including densified and porous types.

Carbon-Graphites

Vitreous (or amorphous) carbon

Diamond

Pyrolytic carbon

Siliconised carbon

Fibres for reinforcing composites, which have a wide range of properties and characteristics, [See also:
Chapter 2; 42.6].

Carbon-carbon composites, [See also: Chapter 54]

Foams

Nano materials, e.g. carbon black (particles); CNT nanotubes; CNF nanofibres, [See also: Chapter
102].

CarbonmaterialsareerroneouslydescribedasgraphiteintheUSA.Inthecontextofthishandbook,
thetermgraphiteisusedonlyforthesoft,hexagonallycrystallised,allotropeofcarbon.

43.10.1.2 Graphite
Graphite is a relatively soft and weak material because of its platelike crystalline structure. It
possesses good selflubricating capabilities, making it useful at temperatures where other lubricants
arenotreliable,e.g.atloworhightemperatures.Inthevacuumofspace,graphitelosesitslubricating
properties and is abrasive. It can however be combined with other lubricants known to perform
correctlyinthespaceenvironment,[See:ECSSQ7071].
Thepropertiesofgraphiteareanisotropiciftheflakestructureisfullyaligned.Notallcommercially
availablegradesofgraphitearealigned,sotheirpropertiesaremoreisotropic.

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Graphite is used in a structural, or semistructural, role in many industry sectors for handling and
processing corrosive chemicals, often at high temperatures, e.g. heat exchangers, large tubes and
vessels,Ref.[4321],[4322].
Apartfromdensifiedformsofgraphite,poroustypesarealsoavailable,e.g.:

Exfoliatedgraphite(alsocalledgraphitefoilintheUSA)isabinderless,flexiblesheetmaterial
produced by expanding an interlocked graphite flake structure by over 100 times in the
thickness direction. The exfoliation process effectively forms an interlocked, porous material
with a layered structure that renders it flexible. The composition is pure graphite with a low
levelofresiduefrommaterialsusedintheexfoliationprocess.Propertiesareanisotropicdueto
thealignmentoflayersparalleltothesurface.Boththeelectricalandthermalconductivityare
highinplanebutlowerfortheoutofplanedirection.Exfoliatedflexiblegraphiteisusedfor
hightemperature gaskets and seals (asbestos replacement) and thermal interfaces. It is also
under evaluation for applications such as electronics (EMI shielding), vibration damping and
applicationsintheelectrochemicalindustries,Ref.[4342]

Carbon foams, which are rigid porous graphitic materials, are under consideration for
spacecraft thermal management systems, Ref. [4323], [4324], [4325]. The properties of the
foams, e.g. density, strength and thermal or electrical characteristics, can be adapted during
manufacturetosuitvariousapplications.

43.10.1.3 Vitreous (amorphous) carbon


Vitreous carbon is a nonporous, amorphous, glassy form of carbon which possesses combined
strength and corrosion resistance. It is rarely used as a monolithic material, except in laboratory
apparatus,butitisamajorconstituentin:

Carbonbased refractories, as a solid matrix phase used to bind graphite flakes or other
constituents,e.g.siliconcarbide.

CarbonGraphites,alsoknownasmechanicalcarbons.

43.10.1.4 Carbon-Graphites
Also known as mechanical carbons, carbongraphites are a combination of amorphous carbon and
graphite. There are a range of materials available, varying in composition of these two phases. The
aim is to produce a material which is strong and hard, but with a low coefficient of friction. Some
grades provide excellent corrosion resistance, whereas others can operate for extended periods at
temperatures above 315C. The maximum use temperature is usually determined by the oxidation
rate in an oxidising environment, e.g. air. In nonoxidising atmospheres (inert or reducing) and
vacuum,themaximumusetemperatureisabout3000C.
Carbongraphites are, in general, chemicallyinert, temperature resistant, lightweight, resilient,
dimensionally stable and impermeable to gases and liquids, Ref. [4319]. Depending on the
processing, some carbongraphite grades can exhibit anisotropic properties, though less so than
pyrolyticcarbons.Inthesegrades,theflakesinthegraphiticphasearealignedtoenablethematerial
characteristicstobedirectionallyoptimised,e.g.conductivitiesandoxidationresistance.
Components can be moulded to shape or machined to size with close tolerances. Items can also be
impregnatedwithavarietyofsubstances,fromresinstometalcompoundstoenhanceperformanceor
permeability. They can be plated, vulcanised to rubber, cemented or shrunkfit into housings or
retainers,Ref.[4319].
Mechanical carbon materials are typically used in a variety of bearings, seals and pumps. Some
examplesofaerospaceapplicationsinclude:SpaceShuttle;MarsLander;aircraftturbineenginemain

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shaftseals(highspeed,hightemperature,cyclicconditions);shaftsealstopreventhotgasesaffecting
bearings.

43.10.1.5 Pyrolytic carbon


Pyrolytic carbon is produced by vapourphase techniques in which the carbon is deposited onto
substrates (CVD). The materials have anisotropic properties, but are stronger than conventional
polycrystallinegraphite.

43.10.1.6 Diamond
Diamond is a wellknown hard, wearresistant material. Natural diamonds are limited by the small
availablesizestoapplicationssuchasprecisionbearingsinsmallequipmentorabrasivesandcutting
tools. Developments in synthetic processing techniques now enable large, simple shapes to be
manufactured rather than just thin films or coatings deposited on substrates. Consequently more
potentialapplicationsnowexist,e.g.opticalandthermalmanagementcomponents,[See:43.17].

43.10.1.7 Siliconised carbon


AlsoknownassiliconizedgraphitesintheUSA,thesematerialshaveasiliconcarbidesurfacelayer
formedbyliquidorvapourinfiltrationprocesses.Comparedwithcarbonalone,theyhaveincreased
hardness, lower porosity and improved oxidation resistance. Similar processes are used to
manufactureceramicmatrixcomposites,[Seealso:Chapter88].

43.10.1.8 Nano materials


Carbonnanomaterialscanbebroadlygroupedas:

Particles in a variety of shapes and sizes, e.g. carbon black which is an established industrial product
commerciallyavailableinmanydifferentgrades,Ref.[4356].

Structures, e.g. CNT carbon nanotubes; CNF carbon nanofibres of various forms and aspect ratios,
e.g.severaltensofnanometresindiameter,severaltensofmicrometerslong.Theirappearance
can be described as platelets, herringbone, screwtype. Papers and foams can be made from
mixtures ofCNT and CNF, Ref.[4353]. All thesematerials are recent innovationsandstillin
theearlystagesofdevelopmentandevaluation,Ref.[4354].

Carbon black is produced by subjecting hydrocarbons, such as heavy residual fueloil feedstock, to
extremely high temperatures in a carefully controlled combustion process. Fine adjustment of the
production process parameters results in a different size and structure of the carbon black and
provides the range of commercial grades. The primary carbon particles are of the order of 12nm to
75nminsize,althoughtheseareprocessedtoformaggregatesthefinestofwhichtendtobemicron
size, e.g. 0.1m to 0.6 m, Ref. [4356]. Carbon black is an established and widelyused industrial
product.Sometypicalapplicationexamplesinclude:

Reinforcing agent in elastomers, e.g. vulcanised rubber products, such as rubber tyres for
vehicles;drivebelts;hoses;gasketsandseals,[Seealso:75.3].

Polymers, e.g. conductive packaging, films, fibres, mouldings, pipes, semiconductive cable
compounds,conductiveresinsandsimilarcompounds.

Coatings,e.g.pigments,provideconductivity,UVprotection.

Tonersandprintinginks.

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Carbon nano materials are essentially extremely fine filler substances that, when added in small
quantities, are seen as a means of enhancing the characteristics of engineering materials by some
amount,e.g.electricalandthermalconductivityofpolymers,ceramics,glasses,Ref.[4353].
Incomposites,incorporatingnanomaterialsofvariouscompositionsaimstoimprovetheperformance
ofthematrixphase,e.g.mechanicalandthermophysicalpropertiesofpolymerresins,Ref.[4355].
[Seealso:Chapter102]

43.10.2 Typical properties


43.10.2.1 General
Table43.10.1comparesthebasicpropertiesof100%carbon,100%graphiteandtwocarbongraphite
materials,Ref.[4318].

Table43.101Technicalceramics:carbontypestypicalproperties
Property
(2)

Apparent density (kg/m3)


Hardness
Compressive strength (MPa)
Flexural strength (MPa)
Modulus of elasticity (GPa)
Thermal conductivity
(W/mC)
Temperature limit (1), in air
(C)
Key:

Carbon
100%

Carbon
graphite
(70%:30%)

Carbon
graphite
(30%:70%)

Graphite
100%

1700
100
300
62
21

1720
85
208
62
17

1750
65
145
52
14

1800
40
55
28
10

12

85

315

315

315

455

(1)Thetemperaturelimitisdeterminedbytheoxidationrateinair;(2)Dependingontheprocessing,
propertiesofcarbongraphitescanbeanisotropicduetothealignmentofthegraphitephase.Non
alignedphasesgivemoreisotropiccharacteristics.

Excluding reinforcement fibres and carboncarbon composites, of the various types of carbons
available,thoseconsideredforaerospaceapplicationsare:

carbon-graphites, which are used in certain load-bearing aerospace applications;

carbon foams, which are under consideration for thermal managementsystemsonspacecraft.

43.10.2.2 Carbon-Graphites
Thepropertiesofsomecommerciallyavailablegradesofcarbongraphitematerialsaresummarisedin
Table43.10.2,Ref.[4319],[4320].

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Table43.102Technicalceramics:carbongraphitegradestypicalproperties

Key

EK 2000

EK 2209

EK 3205

EK 24

Resi
n
-

None

Antimony

None

1820

1770

2250

1700

(2)

2.5 (2)

8.0 (2)

110

110

115

105

137.
9

138

200

200

260

180

55.1

55.2

48

20.7

13.8

12.4

75
27.0

65
26.0

95
30.0

60
18.0

71

14

14

20

14

5.0

3.8

4.0

4.1

Highly loaded seals and


bearings

Highly loaded seals and


bearings

Dry running (3)

MAM&T
P-03

MAM&T
P-7454

Applications(examples)

76

1850

1770

1800

10

90

65

75

90

275.8

179.
3

86.2

2000

2.5 (2)

Rocket nozzle Mars


Lander (initial)
Environmental
recirculating pump on
space station ISS (system
to remove CO2)
Highly loaded seals and
bearings

Hardness (Shore
Scleroscope)
Hardness (Rockwell B,
HR5/100)
Compressive strength
(MPa)
Transverse strength
(MPa)
Flexural strength (MPa)
Youngs modulus (GPa)
Fracture toughness (MPa
m1/2)
Thermal conductivity
(WmK, 20C)
Coefficient of thermal
expansion, 20C to 200C
(10-6 /C)

MAM&T
CJPS

Grain size (m)


Bulk density (fired) (103
kg/m3)
Apparent porosity (%)

Rudder speed brake


assembly on Space Shuttle

Composition (%, typical)


Additions (1)

MAM&T
P-5N

Property

Seal components in
cryogenic pumps in Space
Shuttle main engines

Examplesofcommerciallyavailablecarbongraphitegrades

2.5

MAM&TgradesfromMorganAdvancedMaterials&Technologyandusedinspaceapplications
(stated);SelectedcarbongraphiteEKgradesfromSGLCarbon,forhighloadapplications;(1)
Impregnated;(2)Openporosity,%;(3)Severaldifferentdryrunninggradesavailable.

CarbonGraphite materials are used mainly in sealing and bearing applications, where material
selectioninvolvesconsiderationofloads,speeds,temperatures,matingmaterials,costconstraintsand
projectedvolumes.
Manycarbonbasedmaterialtypesareavailable,withvariousmodificationsforparticulardesignsand
environments, e.g. for high temperatures or corrosive materials.Depending on the particular grade,
carbongraphites can be manufacturedin a variety of shapesandsizes, e.g. cylinders up to530 mm
diameter200mmhigh;platesupto600mm325mm130mmthick,typically.

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Some grades have safety approvals for use within specific environments, e.g. oxidising conditions,
foodcontact,potablewater.

43.10.2.3 Foams
Porousformsofcarbonincludeflexible,exfoliatedgraphite,[See:Graphite]andrigidfoams.
ConductedaspartofanongoingAFRLprogramintheUSA,thepotentialusesofcarbonfoamsin
spacecraftthermalmanagementsystemsisunderevaluationbyNorthropGrummanSpace,Ref.[43
23].
Spacecraft thermal management systems comprising of lightweight, thermallyconductive materials
are considered necessary to accommodate high heat dissipation in military and communications
payloads.Theseapplicationsareincreasinglyusingdenselypackedelectronicsforextendedmission
lives,Ref.[4323].
Optimised designs for spacecraft radiators using carbon foams can potentially simplify radiator
structures. Reducing the need for doublers and heat pipes to dissipate the heat generated by the
electronicswhilstmeeting,orlowering,themassbudgetforthethermalmanagementsystem.
PropertiesofthecarbonfoamsunderconsiderationbyNorthroparegiveninTable43.10.3,Ref.[43
23],[4324].AllthecarbonfoamscitedareofUSorigin.
Thepropertiesofcarbonfoamsareanisotropic.

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Table43.103Technicalceramics:carbonfoamstypicalproperties
Examplesofdevelopmentcarbonfoams
TRLMER
Touchstone Research Corporati
Laboratory
on
CFOAM
25
(3)

Grade (4)
not stated

900

61
95

350

>15

5.5

2.1

5.9

0.84

0.07 to
0.7
0.1 to
100
1.5 to 2
-

0.84

1.4

2.3 to 10.2

25

0.18 to
5.0
5 to 210

150

100 to 125

5.8
-

1.5 to 2
-

245
70
1.02
3.26
1.07
1.31

1.5 to 2
-

Mechanical properties can be


modified
to meet particular applications;
Grade
25 is promoted for composite tooling
High thermal conductivity;
high compressive strength
Panel sizes (approx.):
250 mm 250 mm 25 mm thick.

400

Large sizes available


Panel sizes (approx.):
1.1 m 0.6 m 25 mm thick.

160 to
800
-

Pitch
precurs
or

Pitch
precursor

Uniform microstructure;
high stiffness
Panel sizes (approx.):
400 mm 350 mm 12 mm thick.

500

Bulk density (kg/m3)

Comments

POCO
HTC

160 to
620
-

Coal-based product

Thermal conductivity
(WmK)
in-plane
out-of-plane
CTE, (ppm/K)
in-plane (50C to 150C)
(600C to 800C)
out-of-plane (50C to
150C)
(600C to 800C)

Grade (4)
not
stated

Ultramet

CVD pyrolytic
graphite on
reticulated
vitreous carbon
230 to 610

Composition

Total porosity (%)


Open porosity (% of
total)
Pore size (m, typical
dia.)
Compressive strength
(MPa)
Compressive modulus
(GPa)
Youngs modulus (GPa)

Grade (4)
not
stated

High thermal conductivity;


producible product
Panel sizes (approx.):
250 mm 250 mm 37 mm thick.
Thermal management material; high
thermal conductivity; laminated to
form panels and enclosures; RF
shielding.
Panel sizes (approx.):
300 mm 300 mm 37 mm thick.

Property
(5)

Grade (4)
not
stated

Poco Graphite (1, 2)

Key AllsourcescitedareofUSorigin;POCOFOAMandPOCOHTMaretrademarksofPocoGraphiteInc.(USA);
CFOAMisatrademarkofTRLTouchstoneResearchLaboratory(USA).(1)Licensedmanufacturerof
thermallyconductivegraphitefoamdevelopedbyOakRidgeNationalLabs.(USA);(2)POCOFOAMgrade:
Outgassing(ASTME595):TMLtotalmassloss=0.031%;VCMvolatilecondensiblematter=0.017%;(3)
CFOAMfireresistancepassISO,MILandASTMstandards;(4)Rangeofpropertiesforfoammaterials
fromsource;Ref.[4323];(5)Propertiesareanisotropic

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43.11

Silicon oxide: Silica

43.11.1 Typical characteristics


Silicabasedmaterialsareusuallygroupedaseither:

Fusedsilica,whichisusedforitsthermalshockresistance.

Fusedquartz(vitreoussilica),whichisusedforopticalapplications.

Both types of materials possess low thermal conductivity and high electrical resistivity and are
virtually inert to the majority of aggressive chemicals over a wide range of temperatures. The main
exceptionsare:

HF(hydrofluoricacid),whichreactsatalltemperatures.

Phosphoricacidabove200C.

Causticoxidesreactslowlyatambienttemperaturesbutincreaseswithtemperature.

Someliquidmetals.

Somemetaloxidesabove800C.

Silicabasedmaterialsareavailableas:

castablesandslips,

various standard shapes and forms (tubes, plates, discs), e.g. plate sizes up to 1.2m 0.6m
10mmthick;tubes0.8m1.5mlong.

components.

fibrousforms(insulationproducts),[Seealso:Chapter99].

powders or microspheres, which are used as fillers and additives for other materials, e.g.
pottingcompounds.

nano materials, which areunder evaluation for many variedapplications, e.g.fine particulate
additivesinthepolymermatrixphaseofcomposites,Ref.[4355].

Usesofsilicabasedmaterialsarewideranging,fromcomponentsinmaterialsprocessingindustries
andopticalapplicationstoradomesandnosecones,e.g.Patriotmissilesystem.
For missile nose cones, the design drivers are transparency to various microwave energies, coupled
withmechanicalstrengthtoenablethemissilesystemtowithstanderosionandthelargetemperature
excursionswhileflyingathypervelocitiesthroughtheatmosphere,Ref.[4314].
TheSpaceShuttleOrbiterusessilicaforexternalwindowsandwithintheTPS,[Seealso:71.5].

43.11.2 Typical properties


Table43.11.1summarisesthepropertiesforsomeexamplesofcommerciallyavailablesilicamaterials,
Ref.[4313],[4314].

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Table43.111Technicalceramics:silicatypicalproperties

Key:

99.9999
99.8(1)
2210 (2)
2150

THERMO-SIL
ISOMOLDED (3)

(3)

2005

1970

2020

9
-

10
-

7.5
-

2000

50

207

75.9

18.6

56.2

11.4

37.2

38.2

34.5

2150

74

0.84

0.75

0.62

0.54

0.54

0.6

0.5

0.8

High-precision shapes (materials


process industry); corrosive
environments.

Thin-walled detailed shapes by


shell casting

Shapes (size and mass); Materials


process industry (high-temperature
precision platens, load-bearing
support parts)

Materials processing industries, inc.


semiconductors; electrical
insulators.

Applications
(examples)

99.95

Materials processing industries, inc.


semiconductors; electrical
insulators.

Silica content (%,


typical)
Grain size (m)
Bulk density (fired)
(103 kg/m3)
Porosity apparent (%)
Vickers (GPa, Hv0.5kg)
Rockwell (R45N)
Compressive strength
(MPa)
Flexural strength
(MPa)
Youngs modulus (GPa)
Fracture toughness
(MPam1/2)
Thermal conductivity
(WmK, 20C)
Coefficient of thermal
expansion, 20C to
1000C (10-6 /C)

THERMO-SIL UHS

Property

THERMO-SIL HS (3)

SPECTROSIL

VITREOSIL

Examplesofcommerciallyavailablesilicagrades

VITREOSILandSPECTROSILaretradenamesofSt.GobainQuartz,THERMOSILand
ISOMOLDEDaretradenamesofCeradyneInc.;(1)Rangeofpurities:Highpurity
transparentgrade,puritiesallexceed99%,butvarywithopacity;(2)Transparent
grade;(3)Averagevalues;

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43.12

Silicon carbide

43.12.1 Typical characteristics


43.12.1.1 General
Thegeneralcharacteristicsofdensifiedsiliconcarbideinclude:

Lowdensity,

Hardnessandwearresistance,

Highstrength,

Lowthermalexpansion,

Highthermalconductivity,

Usefulelectronicproperties,

Chemical resistance; good oxidation and hotcorrosion resistance, depending on purity and
processingroute,

ThermalShockresistance,

Hightemperaturestrength,dependingontheprocessingroute,

Thermalstabilitytoveryhightemperatures(2200Cto2800C,dependingonthegrade).

The performance of commerciallyavailable grades of silicon carbide is strongly linked to their


processing routes, which determine the microstructure, e.g. grain size, residual porosity levels and
residual free elements. This, in turn, dictates their mechanical characteristics and hightemperature
environmentalresistance.

43.12.1.2 Processing
The processing routes use various techniques to compact and densify powders or deposit material
fromavapourphase,Ref.[431]:

Hot pressing of pure silicon carbide to produce high density materials needs both a high
temperature and high pressure, e.g. above 2000C at 2 GPa. Additions of alumina or boron
carbidecanreducethepressurenecessary.

Pressureless sintering (moderate temperatures, no pressure) uses fineparticlesize silicon


carbidepowderswithadditionsofothermaterialstoactassinteringaids.

Reaction bonded or sintered materials vary in composition and process details. These are
usually fully dense, but can contain some free silicon. Applications include wearparts and
hightemperature precision components. To improve the hightemperature capability of
reactionbonded materials, a nitriding process to convert any free silicon to silicon nitride
resultsinmaterialsknownasnitrogenbondedsiliconcarbide,Ref.[4347].

Siliconinfiltrated silicon carbide is a process where silicon carbide powder is mixed with
carbon or graphite then compacted into a green shape. Silicon, as either a liquid or vapour
phase, infiltrates the green shape and reacts with the carbon to form silicon carbide which
bonds the silicon carbide particles together. Usually around 10% residual, unreacted, silicon
remains in the densified item. This affects the hightemperature performance, i.e. the melting
pointofpuresiliconisabout1400C.AsimilarprocessisusedtomanufactureCesicinwhicha

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carbon felt rather than carbon powder is used to react with the liquid silicon to form silicon
carbide.

Chemical vapour processes, either CVD deposition or CVI infiltration, rely on the reduction of
siliconandcarboncontainingchemicalsathightemperatures.Thesetechniquesproducehigh
puritysiliconcarbidewithhighoxidationresistance.Depositioncanbeonasubstratetoforma
protective coating, e.g. oxidation protection of porous or nonporous substrate materials;
whereas infiltration can be used to densify green shapes by producing silicon carbide within
interstices. CVI processes are used to create silicon carbidebased ceramic matrix composites,
[See:88.22].

43.12.2 Typical properties


Table 43.12.1 summarises the properties of some commerciallyavailable silicon carbide grades
producedbydifferentprocessroutes,[4312],[4314],[4327].
Of these materials, SiC 100, Cesic and SiC 54 have been extensively evaluated for space
applications,[Seealso:43.18].
TubesofsinteredSiC(Hexalloy)andsiliconinfiltratedcarbonfeltareunderevaluationfortheGAIA
opticalbenchtrussstructure,Ref.[43109].

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Table43.121Technicalceramics:siliconcarbidescomparisonofmaterials
propertiesproducedbydifferentprocessroutes

1300C
Fracture toughness
(MPam1/2)
Thermal conductivity
(WmK, 20C)
CTE, (10-6 /C)

Applications(examples)

Key:

SiC 54S
Isostatic
pressed +
Sintered

CVD (1)

CVD (1)

3150

2000
3000
483
3790
103
449
124
414
-

CERATREX
SC-3P

Cesic
Silicon
infiltration

2900
3100
-

3150

Performance
SiC

SiC 100
Isostatic
pressed +
sintered

CERALLOY
146-IS
Hot pressed

(6)

PUREBIDE

CERASIC

(6)

2 - 10

>3100

2650

3150

3210

3200

<3.5
0

1.5
0

2200
3000
552
2751

2.3
-

2.2
-

2.3
-

2.8
-

2.8
-

3000

2200

450

375

450

>130

365 (2)

450 (2)

375

450

450
450

560 (2)
-

440

420

225

415

450 (2)

440

152 345
-

3.5

2.5

3.5

>4.6

170

115

180

420

4.5

4.8 (5)

4.6 (5)

430

(2)

2.94

(3)

3.1

160

110

250

200

0.003

3.8 (8)
4.4 (9)

4.5 (4)

4.5 (5)
Corrosion resistance; wear resistance; nearnet shape to 400 mm OD.

Youngs modulus (GPa): 20C

2650
3100
-

0% free
Si
5

Corrosion resistance; semiconductor


material process industries

Flexural strength, (MPa):


20C
1300C
1450C

99.3

Space and avionics applications.


Optical and electro-optical systems, e.g.
NIRSpec (JWST).

Compressive strength (MPa)

(7)

Space-destined applications: telescope and


optical system structures and supports. e.g.
NIRSpec (JWST).

Vickers (GPa, Hv0.5kg)


Vickers (GPa, Hv0.3kg)
Rockwell (R45N)

99.9995

Space-destined applications: telescope and


optical system structures and supports. e.g.
ARAGO, Herschel, OSIRIS, ROCSAT, VLTNAOS, SPICA, GAIA, NIRSpec (JWST).

Hardness (Vickers)

99.9995

Corrosion resistance; wear resistance

Porosity (apparent, %)
Porosity (open, %)

Reaction
bonded

Bulk density (kg/m )


3

Pressureless
sintering

Silicon carbide content (%,


typ.)
Grain size (m)

Wear parts; corrosion resistance, e.g.


automotive parts, material process
industries
High friction; high temperature, e.g. fluid
handling, high-speed rotation parts,
aerospace.

Processingmethod

Abrasive; corrosive, e.g. high-pressure,


hightemperature process chemicals-

Property

Self-sintered

PUREBIDE

Examplesofcommerciallyavailablesiliconcarbidegrades

PUREBIDE&HALSIC:MorganAM&T;PerformanceSiC:MorganAdvancedCeramics(CVDDiv.);CERASIC:ToshibaCeramics
Co.;CERATREX&CERALLOY:Ceradyne;SiC100:BoostecIndustries(F);CesicECM(D);SiC54S:Bettini(I);(1)Chemical
vapourdeposition;(2)4pointbendtest;(3)microindentationtest;(4)20Cto950C;(5)20Cto1000C;(6)Rangeofpropertiesfor
variouscommercialgrades;(7)20Kto100K;(8)20Cto400C;(9)20Cto800C.

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43.12.3 Materials for space applications


43.12.3.1 General
The majority of silicon carbide materials are used for their thermomechanical properties.
Applications, depending on the grade, range from refractories to highperformance engineering
materialsandCMCceramicmatrixcomposites,[See:Chapter52].

43.12.3.2 Monolithic ceramics


Inadditiontohightemperatureapplications,thelowthermalexpansioncoupledwithhighstrength
andstiffnessmakesomesiliconcarbidegradesofinterestfordimensionallystablestructures,suchas
ingroundandspacebasedopticalstructuresandsystems.Somegradesofsiliconcarbidehavebeen
extensivelyevaluatedforsuchapplications,e.g.

Cesic

SiC54S

SiC100

43.12.3.3 Foams
Whilst the majority of commerciallyavailable silicon carbide grades are densified materials (low
porosity), some specialist suppliers produce deliberately, openpore materials, Ref. [4328], [4339],
[4359],[4360],e.g.:

Ultramet(USA).

SchaferCorp(USA)

DuocelfromERGMaterialsandAerospaceCorporation(USA)

SiCLigaFillfoamsfromFraunhoferIKTS(D)

Ceramic foams were originally developed as filters for molten metal about 40years ago. During
processing, an open cell structure forms that resembles that of polyurethane foam but in which the
porewalls(knownasligaments)arehollow.Thesehollowwallsaretheninfiltratedtoproducesolid
ligamentsthatprovideasubstantialincreaseinstrength,Ref.[4339].
SiC foams are now considered to have potential uses in space structures as possible replacement
materialsforglassceramicsorberylliumandasacompetitortoconventionalsiliconcarbideusedfor
some large, lightweight mirrors and structures, Ref. [4329], [4339], [4357], [4358], [4359], [4361]
andascoresforsandwichpanels,[Seealso:Chapter26].
The majority pf SiC foams are of USA origin. A summary of properties for Duocel of interest for
sandwichpanelcoresisprovided,[See:Table26.3.7].
WithinEurope,FraunhoferIKTS(D)hasdevelopedSiCLigaFillfoams,Ref.[4339].Highstrength
LigaFillfoamscontainbetween70%and90%pores,withcellsizesintherangeof10to60poresper
inch(4to25porespercentimetre,i.e.porediametersfrom0.4to2.5mm),typically.Fractureloads,
determinedbyindentationtests,areintherangeof900Nto7500N,dependingonthefoamstructure.
Hightemperature resistance is toabout 1300C, Ref. [4339]. Sandwich panels, comprisingof silicon
carbideskins(matorplates)canbeassembledtofoamcoresbyapastetechnique,Ref.[4339].
AnotherproductCeranet,alsodevelopedbyFraunhoferIKTS,isnotfoambutalightweightsilicon
carbidematerialwithanetlikestructure.

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43.12.4 Cesic
43.12.4.1 Introduction
Cesic is high-performance technical ceramic material from ECM (Munich, D). It contains a mixture of silicon
carbide, silicon and carbon phases after processing, Ref. [4357]. The material was evaluated for the
development of the optical bench of the NIRSpec instrument on the JWST James Web Space Telescope,
[See:43.18]andalsomirrorsforNIRSpec,Ref.[4358].

43.12.4.2 Material composition


Cesic uses a felt of short, chopped randomly-orientated fibres as a precursor material. During the hightemperature processing stage, the carbon reacts with liquid silicon to form silicon carbide. Cesic can be
considered a composite rather than a conventional technical ceramic because of the initial fibrous content and
the mixture of resulting phases. The material properties of Cesic are isotropic, whichmakesitmorelikea
conventional technical ceramic than a composite that has anisotropic characteristics conferred by a
continuous fibrereinforcement. The processing stages, which determine the final material
composition and structure, also share similarities with those used in the manufacture of continuous
fibrereinforcedCMCshapedcomponents,[See:Chapter52].

43.12.4.3 Material processing sequence


ThebasicmanufacturingprocesssequenceforCesic is summarised in Figure 43.12.1.

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ECSSEHB3220Part4A
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CARBON BLANK
Carbon felt infiltrated with phenolic resin.
Moulded under pressure to form a blank.
Vacuum heat-treatment.
Carbon blank size: 1100 mm 1100 mm 80 mm

ASSEMBLY OF BLANKS
(bonding)

MACHINING OF BLANKS
(CNC milling and pre-holes)

INSPECTION
(green body)

SILICON INFILTRATION
[See: Figure 43.12.2]

1600C process temperature


Vacuum
Transformation of Si to SiC by reaction with carbon (matrix and fibres)
Capacity: 2.4 m diameter; three 1.2 m levels

EXCESS SILICON REMOVAL


(sand-blasting)

INSPECTION
(cracks; geometry)

FINAL MACHINING
EDM technique
Grinding (diamond tools)

FINAL INSPECTION
Non-destructive test (dye penetrant; ultrasonic)
Geometry
Mass

Figure43.121Cesic:Basicprocessingsequence
The Cesic process is known as directtoshape because the carbon greenbody shape is produced
closetothefinalsizeandshapeofthefinalstructure.
Directtoshape implies better dimensional control than other processes described as nearnet
shape.
During the infiltration process, the transformation from carbon to silicon carbide that occurs is a
solidtosolid reaction; hence no deformation occurs due to effects such as gravity. Whereas some
ceramics, processed by different methods, exhibit large dimensional changes during manufacture,

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Cesic undergoes a low, controlled shrinkage of only 0.2%. This enables closetolerance structural
partstobeproducedandreducestheneedformachining.
Dependingontheparticularstructurebeingmade,additionalprocessescanbeused,Ref.[4357],e.g.

mirrors, which have a surface preparation step prior to coating and a polishing stage after
coating.Theopticalqualityisalsoestablishedduringthefinalinspection.

small components do not always need assembly of multiple carbon blanks; maximum blank
thickness80mm.

large structures can be produced as subassemblies, which are then joined after silicon
infiltration,finalmachiningandinspectionsteps.

43.12.4.4 Process equipment


Theinfiltrationfurnace,installedatECMinGermany,isshowninFigure43.122.Thisequipment
enablesinfiltrationofcomponentsupto2.4mdiameter.
Heater unit

Cesic silicon infiltration facilities at ECM (Munich, Germany) capable of processing up to 2.4 m diameter structures.

Figure43.122Cesic:Siliconinfiltrationprocessingequipment
43.12.4.5 Machining
EDM and wire erosion machining is possible because Cesic is electrically conductive. The EDM
technique offers a number of advantages over grinding, e.g. fast and accurate, so less expensive. For large areas,
the tolerances achievable are flatness <10m; position 20m. Combining wire erosion machining
(preliminary)withEDM(finishing)achievestolerancesof10m for an 7mm hole.

43.12.4.6 Material characteristics


The material properties were determined during the designdevelopment of an optical bench; a
dimensionallystable structure for the JWST/NIRSpec programme, [See: 43.18]. Properties, related to
itspotentialuseformirrorsforNIRSpec,werealsoestablished,Ref.[4358].
Thematerialpropertiesareisotropicandarenotaffectedbytheprocessingconditions,e.g.infiltration
runsordirection,andarealsoindependentofsurfacecondition.
The properties are reproducible between different production runs using different batches of green
bodycarbonblocks;asdemonstratedbytestsonsamplestakenfromdifferentmaterialbatches.

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Isotropywasdemonstratedbysamplestakenfromdifferentorientations,i.e.samplesdenotedasx,y
andzdirections.
Thetestsconductedincluded,Ref.[4357]:

coefficientofthermalexpansion,fromRTto20K

4pointbendingtoanASTMstandard.

Biaxialtest,atRTandlowtemperature(liquidnitrogen).

43.12.4.7 Mechanical properties


Table43.12.2summarisesthemechanicalpropertiesofCesic. The 4-point bending tests use two different
sample sizes; both of which are relatively large compared with those used often used for ceramic material test
campaigns.

Table43.122Cesic:Mechanicalproperties
Property(1)
Density

(kg/m3)

Value
2650

Comment
Ref. [4357]

Modulus, E (GPa)
Specific bending stiffness, E/ (MPa)
Strength (MPa)
Fracture toughness, KIC
Bending strength, at RT (MPa): large
sample:

225
>13.7
>130
>4.6

Mean
Maximum
Minimum
SD
Weibull
Bending strength, at RT (MPa): small
sample:
Mean
Maximum
Minimum
SD
Weibull
Directionality (bending strength):
x-direction (MPa)
y-direction (MPa)
z-direction (MPa)
Bi-axial bending strength, at RT, (MPa)
SD
Bi-axial bending strength, at LN2 temp,
(MPa)
SD
Key:
(1) SD standard deviation;

111.1
152.3
80.7
15.7
11

ASTMC1341
(150mm 30 mm 3mm);
97 samples tested, Ref. [4357].

148.9
171.6
128.1
13.0
13.6

ASTMC1341
(80mm 30 mm 3mm);
21 samples tested, Ref. [4357].

147.4
151.3
146.9
164.2
22.2
162.9

4-point bending strength,


small sample, Ref. [4357].

(2)

20.4

Ref. [4357]
Preliminary tests, Ref. [4357].

(2) ExInertia/M ratio higher than other advanced materials, d = 2.65

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43.12.4.8 Thermal properties


Table 43.12.3 summarises the temperaturerelated properties of Cesic. The CTE of Cesic is near
zerooverawidetemperaturerange;downtocryogeniclevels.

Table43.123Cesic: Thermal properties


Property(1)

Value

Coefficient of thermal expansion, (106/C):

from 20K to 100K

<0.003

Comment

Michelson
interferometry
technique, 15 samples
tested

Thermal conductivity (W/mK):


at 300K
at 40K

160
35

TheresultsofCTEtestsonmaterialsproducedfromthreedifferentbatches,i.e.infiltrationofdifferent
batches of carbon, and tested in different directions are shown in Figure 43.12.3, Ref. [4357]. The
average value determined from the curves is 238.6m/m with a maximum variation of 5.3m/m at
20K.
Thesamplesforzdirectiontestswerejoinedpriortosiliconinfiltrationbecausethethicknesslimitof
thecarbonblankis80mm(testsamplesize:250mm30mm10mm).
GiventhattheCTEinthezdirectionarethesameasthoseintheotherdirections,wheresamplesdid
notcontainjoints,thisshowsthatthejoiningmethoddevelopedbyECMdoesnotaffectthematerial
expansionorcontractioncharacteristics.

CTEmeasurementon15samplesfrom3batchesofmaterialstestedinx,yandzdirections,wherez
directionsamplescontainedjointsmadepriortosiliconinfiltration.

Figure43.123Cesic:Coefficientofthermalexpansion

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43.12.4.9 Applications: Panels


The combination of the material characteristics and the nearnetshape manufacturing process of
Cesicenablebothstructuralshapesandintegrated,complexshapedassembliestobeproduced.
For example: Ibeams for rigidity, large thin webs (less than 1.5 mm thick) and plates, along with
openbackedstructures,flatorcurvedpanelswithhighdimensionalsurfacetolerances.
Suchstructuraldesignsaretypicalofthoseusedfordimensionallystablestructures,suchasmirrors
andsupportstructures,opticalbenchesorothersimilarequipmentsupports.
Figure43.12.4showsanexampleofa1m2integrallystiffenedpanelmadeofCesic.

Figure43.124Cesicceramic:Exampleofintegrallystiffenedpanel
43.12.4.10

Applications: Mirrors

An ESAfunded study compared Cesic with Bettini SiC-54S for the types of mirrors envisaged for the
NIRSpec programme, [See also: SiC-54S]. Not only the materials were evaluated, but optical coatings,
manufacturing of test mirrors and performance at cryogenictemperatureswerealsoinvestigated,Ref.[43
58].

43.12.4.11

Applications: Optical bench

In the designdevelopment of NIRSpec, an optical bench demonstrator component measuring


1045mm 600mm 100mm was manufactured successfully, [See: 43.18]

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43.12.5

SiC 54S

43.12.5.1 Introduction
ProducedbyBettiniinItaly,SiC54hasbeenevaluatedfordimensionallystablespacestructures.
An ESAfunded study compared Bettini SiC54 with ECM Cesic with for the types of mirrors
envisagedfortheNIRSpecprogramme,Ref.[4358].

43.12.5.2 Material composition


Therawpowderisaspraydried-SiC (Norton standard product) containing>97.7%SiCwith<0.04%free
Sialongwithothermaterialsandtraceelements.Eachbatchofrawpowderissubjectedtoincoming
quality control to determine chemical and thermal analyses, humidity and physical features of
powder,e.g.particlesizedistribution,surfacearea.

43.12.5.3 Material processing sequence


Figure43.12.5summarisestheoverallmanufacturingprocessforSiC54Sfromincomingrawmaterial
tofinalinspectionoffinisheditem,Ref.[4363].Eachstepintheprocessisaccompaniedbyrigorous
qualitycontrolprocedures.

Figure43.125SiC54Sceramic:Processsequence
ThebasicprocesswasusedtomanufacturetestmirrorsfortheNIRSpecprogramme.Toimprovethe
surface polishing capability, a coating was applied to the surface to meet NIRSpec microroughness
demands,Ref.[4358].
Snecmasproprietaryisothermalchemicalvapourinfiltration(ICVISiC)coatingprocesswasusedto
depositadense,homogeneousSiClayerontheSiC54substrates.Theprocessisconductedatalower
temperaturecomparedwithotherchemicalvapourprocesses,Ref.[4358].

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43.12.5.4 Process equipment


Compactionofthepreparedpowdertoformagreenshapeisaccomplishedbywetbag,coldisostatic
pressing.Thegreenshapeisdensifiedbysinteringat1965C in an inert (argon) atmosphere. The sintering
process is accompanied byawitnesssampleforqualitycontrolpurposes.

43.12.5.5 Machining
Prior to densification by sintering, machining is carried out on the green body either after the cold
isostaticpressingstep(turning)orafterthedebindingstep(milling).

43.12.5.6 Material characteristics


The good stability, low shrinkage and low residual porosity of SiC54S make it of interest for optical
applications.

43.12.5.7 Mechanical properties


The mechanical properties of SiC54S are summarised in Table 43.12.4. The values stated are a
combinationofmanufacturersdataandthosedeterminedduringtheNIRSpecmirrorstudy,Ref.[43
58],[4363].

Table43.124SiC54S: Mechanical properties


Property

Teststandard

Value

Porosity:
Open (%)
Closed (%)
Bulk density (g/cm3)
Flexural strength, 4-point, (MPa)
Batch 1
Batch 2
Pf (1) = 63.21%
Bending strength (4-point)
Specific strength, /
Allowable strength, adm
Compressive strength (MPa)
Youngs modulus (GPa):
Specific stiffness, E/
Allowable modulus, E adm
Hardness, Vickers HV 0.5 (GPa)
Fracture toughness, KIC (MPa m1/2)
Weibull modulus
Poissons ratio
Allowable Poissons ratio, adm

EN 623-2
EN 843-1
EN 843-1
EN 843-1
DIN 51067T1
ENV 843-2
ENV 843-4
DIN 51109
ENV 843-5
ENV 843-2
-

0
1.5
3.15
365
369.5 61.4
364.1 64.7
390.28
225 (4)
71
82 (3)
2200
415 1.7 (2)
132
400 (3)
2.3
4
7
0.15 0.001 (2)
0.16 (3)

Key: (1) Pf probabilityoffailure;(2)Basedon3samples;(3)Mirrordesignvalue;(4)


Correspondsto63%Pf probabilityoffailureonincreasedloadarea3200mm2.

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43.12.5.8 Thermal properties


The thermal properties of SiC54S are summarised in Table 43.12.5. The values stated are a
combinationofmanufacturersdataandthosedeterminedduringtheNIRSpecmirrorstudy,Ref.[43
58],[4362].

Table43.125SiC54S: Thermal properties


Property

Teststandard

Value

EN 821-2
EN 821-1

110
130
48

EN 821-1
EN 821-1
(1)

3.8
4.4

(1)
(1)
(2)
(2)
(2)
(2)
(2)
-

2.2
1.0

Thermal conductivity (W/mK):


20C
300K
100K
Coefficient of thermal expansion (106/C):
20C to 400C
20C to 800C
Coefficient of thermal expansion
(ppm/K):
RT
RT to 35K
Heat capacity (J/kg K):
300K
200K
100K
35K
Max. service temperature (C)
Key:

660
392
106
2
1300

(1)MeasuredbyMichelsonInterferometrytechnique(GalileoAvionica,Italy);(2)Special
testfixtureformeasuringthermalcapacitybetween4Kand293K.

43.12.5.9 Applications: Mirrors


Figure43.12.6showstheSiC54SICVISiCcoatedmirrorprototypedesigntomeettheNIRSpecdesign
requirements,Ref.[4358]:

Firsteigenfrequency:>300Hz

Mass:<1.5kg,includingrearmountcollar

Designload:50g(30gsimultaneouslyalongdirections(+x,+y,+z)or(+x,+y,z).

Operatingtemperature:35K,withqualifications20K.

Themirroris170mmdiameter,witharearintegralmountingcollar.
Themirrorsurfaceissphericalwitha600mmradiusofcurvature.Theopenbackfaceofthemirroris
flatwithadepthattheedgeof30mm.Thecellsareequilateraltriangles.

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Figure43.126SiC54S:NIRSpecprototypemirror

43.12.6

SiC-100

43.12.6.1 General
As of August 2004, CoorsTek (USA) and Boostec (France) have a licensing agreement that covers a
wide range of design, processing and manufacturing technologies associated with silicon carbide
mirrorsandstructuralsystemsforopticalapplications,Ref.[4327].Thisincludeshighperformance,
spacebasedtelescopesforearthobservation,astronomyanddefence.Someexamplesinclude:

HERSCHEL (Demonstrator breadboard, Primary mirror)

ROCSAT 2

ROSETTA

OWL

FIRST

ALADIN

ARAGO

NIRSpec James Web Space Telescope (Optical bench, Optical assembly)

VLT-NAOS

GAIA

43.12.6.2 Source
SiC100 has been developed by EADS Astrium SAS together with the manufacturing company Boostec S.A.,
France.

43.12.6.3 Chemical composition


SiC100 is coldisostatically pressed, sintered monolithic silicon carbide, Ref. [43110]. The crystal
structureofSiC100isthealphaform,withcarbonatomsinanhexagonalgridandthesiliconatoms

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occupy the tetrahedral sites of thestructure. The materialis polycrystallineand fullyisotropic. The
meangrainsizeisabout5m.
Keyadvantagesfortheproductionofhighperformancecomponentsorsystemsinclude:

NearlypureSiC,nosecondaryphase.

Isotropicphysicalproperties.

Highmechanicalstrengthandstiffness,insensitivitytomechanicalfatigue.

Highthermalconductivityandlowthermalstrain.

Highstability.

Highresistancetoaggressiveenvironments.

43.12.6.4 Material processing sequence


The manufacturing of SiCparts and components from powder is a wellestablished and qualified
process,comprising:

SiCpowderpreparation,

Isostaticpressing,

Greenforming,alsocalledgreenmachining,

Sintering,

Grinding,

Milling,

Polishing,

Inspection.

Figure43.12.7showsthestepbystepSiC100productionprocess,Ref.[43111].

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Reproduced courtesy of EADS Astrium GmbH

Figure43.127SiC100:ProductionprocessschematicforHerschelprimary
mirror
43.12.6.5 SiC powder preparation
Sinteredsiliconcarbide(SiC)rawmaterialisproducedbymixinghighpuritySiCwithsinteringaids
and binder additives which aid production of largescale products from this finegrained material.
Initially, the powder is ball milled to a precise submicron size distribution. The sintering aids
compriselessthan1%byweightofthesinteredmaterial.

43.12.6.6 Isostatic pressing


Theprocessinvolvesfillingasealablecontainer,suchasarubberbag,withSiCpowder.Therubber
bagisusuallysupportedbyaskeletalstructure,typicallyasteelbox,withperforationsenablingaccess
bytheisostaticpressuremedia,generallywater,tothefullsurfaceareaofthebag.Thisassemblyis
placedintoapressurevesselwhereitissubjectedtohydraulicpressureofabout2100bars.

43.12.6.7 Green forming (green machining)


This process, using CNC machine tools, provides nearnet shaping of non sintered SiC to its final
design. Nearnet shaping in the green state is generally used because SiC can be machined 20 to 30
times faster compared with the fired state. Features can be machined in the green state if their
tolerances for linear shrinkage are in the range 0.2% to 1%. There are a few limitations on the green
forming of SiC-100. The material in the pressed state is friable. It has the mechanical strength of chalk, being
quite brittle and low in strength.Maintainingmachinetoolsiscrucialfortheaccuratemachiningoflight
weightstructures.Aspectratios(heighttothickness)approaching80to1havebeenachievedforlight
weightribs.Advancedmachiningtechniquesusinghighspeed(upto20,000rpm)3and5axismilling
headswithharmonicallyoptimisedtoolshavesignificantlyreducedmachiningtimes.

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43.12.6.8 Sintering
Sintering techniques have improved dramatically in the last 30 years. New furnace technology with
computer controlled zones, optimised gas flow, and vacuum environments now enable sintering of
very large and complex products. The challenge is to produce a uniform temperature during the
sintering process that peaks in excess of 2100C whilst maintaining an environment which removes
binders and prevents oxygen exposure. SiC powder is kept under vacuum or an inert atmosphere
duringtheentiresinteringprocesstoavoiddegradation.Thesinteringprocesstypicallytakesbetween
20hoursand120hours,dependingonthesizeandcomplexityoftheload.
Duringtheprocess,thereare3basicstages:binderburnoutupto500C,densification(shrinkageof
about20%)upto2100C,thencooldown.Theprocessneedstobecontrolledprecisely.Notreaching
the full sintering temperature for the required time can produce a part that is not fully dense.
Exceeding the sintering conditions cancause excessive grain growth, which could be detrimental to
materialproperties.

43.12.6.9 Grinding
GrindingofsinteredSiCissimilartogrindingofothertypesofceramicmaterials.Abrasivediamond
wheelsaresuitabletoolsforthepurpose.Typically,grindingisdonewithalargeflowofwaterbased
coolant to prevent excessive heat. For optical applications, grinding is avoided in order to maintain
the ultimate strength of the material measured in the as fired surface condition. As with most
ceramics,grindingcancausesubsurfacedamagethatcanlowerthestrength by50%ormorewhen
comparedwithanasfiredorhighlypolishedsurface.However,lappingandpolishingoperationscan
removethedamagecausedbygrindingandsorecoverthestrength.

43.12.6.10

Milling

Design details such as interface attachment holes and recessed mounting surfaces are milled in
accordancewithprecisegeometricanddimensionalrequirements.CNCmillingmachineswithupto5
axes are generally used to perform these operations. Machining times for these operations are
relativelylong.Onlydiamondtoolingwithsubstantialcoolantiseffectiveformilling.

43.12.6.11

Polishing

MostopticalpolishingtechniquescanbeappliedtoSiCoptics.Conventionalabrasivepolishingwith
pads and pitch along with advanced techniques such as computercontrolled polishing, ion beam
figuring and magnetorheological finishing have been demonstrated. Diamond is the only abrasive
mediumthatiseffectiveinpolishing.Optimisedremovalratescanbecomparablewithremovalrates
formoretraditionalopticalsubstratematerials.

43.12.6.12

Inspection

Several inprocess and final inspection steps are applied to SiC100 optical projects. Although some
special products are subject to designspecific testing and qualification requirements, the usual
inspectionstepsare:

Greenbodyqualification:Therawmaterialisqualifiedbyusingtestcouponsfordensity,pore
distributionandstrength.

Aspressed blank: The blank is visually inspected for cracks and measured for dimensional
accuracy.

Assintered part: The sintered part undergoes a dye penetrant inspection for cracks and
porosity.

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Ground /machined parts: Dye penetrant inspection for cracks. Dimensional and geometrical
inspectionmeasurements.

Prooftesting:Finalpartscanundergoprooftestingand/orvibrationtestingpriortointegration
intotheopticalsubsystem.

Table 43.12.6 summarises the manufacturing size constraints (as of 2006). It gives the practical size
limitations,determinedbyavailableprocessfacilities,intermsoffinishedpartsize,i.e.aftershrinkage
andmachining,Ref.[43111].

Table43.126SiC100:Manufacturingsizeconstraintspracticalsizelimitations
forfinishedpart
Process

Isostatic pressing
Green machining
Sintering
Grinding
CVD SiC
Brazing

Sizelimitations(m)

Cylindrical:
Rectangular:
Rectangular:
Cylindrical:
Rectangular:
Rectangular:
Cylindrical:
Rectangular:
Cylindrical:
Cylindrical:

1.0
1.0 1.7
0.6 2.0
1.5
1.0 3.0
1.4 1.8
3.5
1.0 5.0
1.5
3.5
(Status2006)

43.12.6.13

Material properties

Material properties are given in Table 43.12.7, Ref. [43110]. Typical characteristics of SiC100 are
statedontheBoostecwebpage.

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Table43.127SiC100:Typicalcharacteristics
Typicalcharacteristics
Chemical
Physical

Thermal

Free Silicon
Crystal structure
Mean grain size
Total porosity
Open porosity
Apparent bulk density
Theoretical density
Coefficient of thermal expansion
Thermal conductivity
Specific heat

Mechanical

Electrical
Service

Conditions

Weibull modulus
Compressive strength
Young's modulus
Shear modulus
Poisson's ratio
KIC toughness
Electrical resistivity
Maximum working temperature

Value

500 g load

wt %
10-6 m
vol %
vol %
kg / m3
kg / m3
10-6/C
10-6/C
10-6/C
W/m K
W/m K
W/m K
J/kg K
J/kg K
J/kg K
C
GPa

20C

MPa

450

1000C
1400C
20C

MPa
MPa
MPa
GPa
GPa
MN m-3/2
Ohm m
C

450
450
10
3000
420
180
0.16
3.5
105
1450

1800

20C to 500C
20C to 1000C
20C to 1400C
20C
500C
1000C
20C
500C
1000C

Maximum thermal shock


Vickers hardness
Mechanical strength (3-point
bend)

Units

20C
Air
Inert
atmosphere

0
alpha SiC
5
< 3.5
0
3100
3210
4.0
4.6
5.2
180
68
40
680
1040
1180
325
22

Status: (30.05.2006)

43.12.6.14

Outgassing

Theresultsofoutgassingtests,conductedinaccordancewithECSSQ7001andECSSQST7002,are
giveninTable43.12.7,Ref.[43112].

Table43.128SiC100:MicroVCMtestE544outgassingvalues
SiC-100

TML(%)

RML(%)

CVCM(%)

0.01

0.00

0.00

ThemeasuredoutgassingpropertiesofSiC100werewithinthosestatedinECSSQST7002.NoFTIR
spectrumwasfoundfromthecondensedmaterial.

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43.12.6.15

Assembly technologies

Conventionalprocesses,suchasadhesivebondingwithepoxyorusingmechanicalfasteners(bolting),
areusedtoassembleSiCparts.Thesetechnologiesoffermicrometricstabilityperformancesufficient
formoststructuralapplicationsorfixings.
Formirrordevelopment,thestabilitydemandismuchmoresevere,soothersprocessesareused.Two
differentassemblytechnologiesforSiC100havebeenachievedinparallel,Ref.[43111],[43113]:

Ceramic bonding.

Brazing.

Bothoftheseassemblymethodsarenowwellestablishedorqualifiedforspaceuse.

43.12.6.16

Ceramic bonding

Ceramicbondingisaprocessthatenablesassemblyofseparategreenbodypartsbeforesinteringto
produce a pure SiC item at the end of the process. The technique uses adhesive containing SiC
particlestobondthetwogreenbodiestogether.Greenbodymachiningofthefullassemblycanthen
proceedintheusualmanner.
Aftersintering,amonolithicSiCpartisobtainedandthebondedinterfacecanhardlybedetectedwith
thenakedeye.Thistechniqueneedsmillingandsinteringfacilitiescapableofhandlingthefinalitem
dimensions. The maximum size that can currently be manufactured is about 1.5 m in diameter. An
exampleofaproductjoinedbyceramicbondingisthe1mdiameterDemonstrationMirror.

43.12.6.17

Brazing

For larger monolithic pieces, brazing is the best solution. The brazing process enables of a large
numberofsinteredSiCpartstobejoinedinasinglestep.Thepiecestobebrazedarepositionedusing
jigs. During the process the braze material fills the gap between the pieces by capillary action. The
operationiscarriedoutathightemperatureunderanonoxidizingatmosphere.Thethicknessofthe
brazedjointsistypicallyaround50m.
Themajoradvantagesofbrazingaretheeaseofprocessingandtheabsenceofanydistortionarising
fromthebrazedjointsduringservice.TheentireassemblybehavesasifitwasmadeofasingleSiC
element. Limited by the dimensions of available brazing furnaces, the maximum size that can
currently be achieved is about 3.8 m in diameter, e.g. 3.5 m diameter for the HERSCHEL primary
mirrormadeof12brazedsegments.
Examples:

HERSCHEL Demonstrator Breadboard.

HERSCHEL primary mirror.

NIRSpec Optical Bench for James-Webb-Space Telescope (JWST).

43.12.6.18

Design guidelines

SomegeneraldesignguidelinesforthemanufacturingofSiC100componentsare,Ref.[43111]:

Thickness>0.5mm,<20mm.

Keepthicknesstransitionstolessthanan8to1ratio.

Webthicknessminimum0.5mmwithaspectratio(heighttothickness)lessthan80to1.

Exteriorchamfers0.5mmto2mm.

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Fillets>1.5mmforbottomofpockets.

Fillets>3mmforvertical.

Asfired(nopostsintermachining)1%lineartoleranceforpocketsandnoncriticalfeatures.

Actual product design parameters have many factors that determine the prudent design rules. An
optimaldesignisachievedbyevaluationonacasebycasebasis.

43.12.6.19

Applications: 1m diameter Demonstration Mirror

A 1 m diameter Demonstration Mirror, shown in Figure 43.12.8, was manufactured for visible
wavelengthapplications,withtwoimportantrequirements,Ref.[43113]:

Lightweight

Representativeoftheactualneedsofopticaldevices,inordertodemonstratethefeasibilityof
largediametermirrors.

Reproduced courtesy of EADS Astrium GmbH

Figure43.128SiC100:1mdiameterDemonstrationMirrorreadytopolish

ThevisiblewavelengthrangeimpliesthataSiCCVDchemicalvapourdepositionlayerisnecessary
beforepolishingandcoatinginordertoachievethedesiredsurfaceroughness.
The 1 m mirror has a concave parabolic shape (primary reflector of Cassegrain telescope). The rear
sideislightweight.Itisanoptimisedopenbackstructure,whichistheeasiestwayofmachiningthe
sinteredSiCblank.
Themirrorwasmanufacturedfromgreenpartsthatarejoinedinthegreenstatebyceramicbonding,
asshowninFigure43.12.9.

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Reproduced courtesy of EADS Astrium GmbH

Figure43.129SiC100: 1m diameter DemonstrationMirrorgreenpartjoining


byceramicbonding
Otherfeaturesofthefinalmirrorare,Ref.[43113]:

15.3 kg mass after grinding, equivalent to less than 20 kg/m with lateral interfaces. An optimisation of
supporting points by analysis enabledamassreductionof50%.

Stiffness of the mirror over 280 Hz (mirror alone) and 175 Hz with supporting devices.

20 g static load, design for sine, random and acoustic environment.

Design for visible wavelength WFE 32 nmRMS.

43.12.6.20

Applications: 1.35 m HERSCHEL Demonstrator Breadboard

The brazing technique for joining was successfully verified by manufacturing of the HERSCHEL
DemonstratorBreadboard,whichiscomposedof9singlesegments,asshowninFigure43.12.10,Ref.
[43113].

Reproduced courtesy of EADS Astrium GmbH

Figure43.1210SiC100: 1.35 m diameter HERSCHEL DemonstratorBreadboard


beforeandafterbrazing
The manufactured monolithic mirror was successfully tested in vibration and low temperature
environment (110 K). The vibration levels were 29 g in lateral direction and 27 g in axial direction.

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Duringthethermaltest,nodistortionresultingfrombrazingorfromCTEvariationbetweensegments
wasmeasuredwithinanaccuracyof0.3m,Ref.[43113].
Owingtothethinnessofthebrazedjoint,ithasnoinfluenceonthepolishingprocessanddoesnot
create any discontinuity. Brazed pieces have been polished without problems even for optical
accuraciesinavisiblewavelengthapplication.

43.12.6.21

Applications: 3.5 m HERSCHEL Primary Mirror

The 3.5 m diameter primary mirror blank for the HERSCHEL telescope was fabricated by brazing
together12siliconcarbide(SiC)segments,asshowninFigure43.12.11,Ref.[43113].

Reproduced courtesy of EADS Astrium GmbH

Figure43.1211SiC100:3.5mdiameterHERSCHELPrimaryMirror
manufacturedbybrazing12SiCsegments
Toprovidemechanicalstability,temporarystiffeningribswerepositionedontheinternalsurfaceof
thesegment,bothduringthemanufacturingofthesegmentsandwhilstthemirrorblankwasbeing
assembled. These were in addition to the external surface stiffeners that are part of the final mirror
configuration.
Oncetheassemblyprocesswascompleted,themirrorblankwasmachinedbygrindingtoremovethe
temporary stiffening ribs, to reduce the thickness of the mirror shell to 3 mm, and to achieve the
correct shell profile ready for polishing, as shown in Figure 43.12.12, Ref. [43113]. The machining
processreducedthemassofthemirrorblankfrom720kgto240kg.

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Reproduced courtesy of EADS Astrium GmbH

Figure43.1212SiC100:3.5mdiameterHERSCHELPrimaryMirrorafter
assembly
43.12.6.22

Applications: NIRSpec Optical Bench Breadboard

During a preparatory technology development activity for the JWST NIRSpec instrument, a
technologydemonstrator(theOpticalBenchBreadboard)wassuccessfullymanufacturedandtested,
Ref. [43114]. Objectives were to manufacture and test an optical bench breadboard model,
representativeindimensions,shapeanddesign,fortheactualsizeNIRSpecinstrumentopticalbench.
Thestudyobjectiveswereto:

validatethecompletemanufacturingsequenceincludingjoiningbybrazing,

demonstratethefeasibilityoftheallceramicSiCconceptforoperationat30K,

providedesignfiguresfortheactualNIRSpecbenchdesign.

Figure43.12.13showsthesuccessfullytestedOpticalBenchBreadboard,whichwasmanufacturedin
SiC100intwohalvesthenjoinedbybrazing.

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Reproduced courtesy of EADS Astrium GmbH

Figure43.1213SiC100:NIRSpecOpticalBenchBreadboard
43.12.6.23 Applications: NIRSpec Optical Assembly for James Webb Space
Telescope
NIRSpecnearinfraredmultiobjectspectrographisoneofthreeastronomicalinstrumentsonboard
the future James Webb Space Telescope (JWST). Its configuration, shown in Figure 43.12.14, is a
dispersive spectrograph capable of observing astronomical objects in the 1 m to 5 m wavelength
range,Ref.[43115].

Reproduced courtesy of EADS Astrium GmbH

Figure43.1214SiC100:OpticalAssemblyofNIRSpecforJamesWebbSpace
Telescope
The NIRSpec optical bench is a large planar structure (1.8 m 1.25 m) made of SiC100. It carries
mirrors,filters,mechanismsandtheFocalPlaneAssembly.AuniquefeatureoftheSpectrographis
its athermal design, where most of its components, particularly mirrors, mechanisms and structure,
aremadefromthesamematerialinordertoavoiddistortionresultingfromthermoelasticmismatch.
Thelargebaseplateisajoinedstructuremanufacturedfromtwomonolithicpartsbrazedtogether.

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43.12.6.24

Applications: High precision components

OtherhighprecisioncomponentsmadeofSiC100forspaceapplicationsaredescribedontheBoostec
website.

43.13

Silicon nitride

43.13.1 Typical characteristics


43.13.1.1 General
Thegeneralcharacteristicsofsiliconnitrideinclude:

highstiffness,

lowthermalexpansion,

goodcreepresistance,

goodthermalshockresistance,

notelectricallyconductive(pure).

Siliconnitridecanbeusedupto1500Cinvacuum.Itdisassociatesat1850Cinnitrogenatmospheres.

43.13.1.2 Sialon
Sialonisamodifiedformofsiliconnitrideinwhichaluminiumandoxygenaresubstitutedforsilicon
and nitrogen to produce silicon aluminium oxynitride. In general they possess good strength,
fracture and wear resistance. Applications include wear parts and hightemperature engine
components.Theadditionoftitaniumcarbideproducesconductivesialons.

43.13.1.3 Processing
Theperformanceofcommerciallyavailablesiliconnitridegradesisaffectedbytheprocessingroute.
This determines the microstructure, e.g. grain size, residual porosity levels, secondary phases, and
consequently the mechanical characteristics and hightemperature resistance. The characteristics of
siliconnitridematerialsproducedbydifferentprocessingroutescanbesummarisedas:

Sintered materials can have strengths approaching those of hot pressed variants and shaped
parts can be made that are not possible by hot pressing. Modified compositions can increase
toughnessattheexpenseofstrength.

RBSN reaction bonded silicon nitride, or reaction sintered, are usually porous and have
moderate strengths but high thermal shock resistance. Uses tend to be for refractories,
exploiting their nonwetting by molten metals. Modified processing can produce fine, even
dispersionsofporosityimprovingthestrength.

Hotpressed or hotisostaticallypressed materials have very high strengths, good fracture


toughnessandgoodoxidationresistance(to1200C).Creepresistancedependsonthepresence
ofglassy,secondaryphases.Usesincludeprecisionhightemperatureengineeringcomponents,
e.g.gasturbineandengineparts.

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43.13.2 Typical properties


Table 43.13.1 compares the properties of some commerciallyavailable silicon nitride materials
producedbydifferentprocessroutes,Ref.[4312],[4314],[4331].

Table43.131Technicalceramics:siliconnitridescomparisonofmaterials
propertiesproducedbydifferentprocessroutes

Dynacer
SSN

SSN
(MAC SSNS)

RBSN (1)
(MAC RBSNS)

CERALLOY
147-01B

Dynacer
RBSN

CERALLOY
147-31N

CERALLOY
147-5

Examplesofcommerciallyavailablesiliconnitridegrades

sintere
d

sintere
d

reactio
n
bonded

reactio
n
bonded

reactio
n
bonded

sintered
reaction
bonded

hot
pressed

Property
Processingmethod
Silicon nitride content
(%, typ.)
Grain size (m)
Bulk density (kg/m3)

99

99

72

92

>98.5

3250

3200

2300

2500

3200

3300

Porosity apparent (%)

2500
20
(open)

16

1500

800

1100

1800

1800

2000

>3000

650

550

200

190

190

700 to 800

930

Key:

290

280

170

175

170

310

320

8.0

2.5

3.0

6.0

6.0

25

15

12

14

16

26

35

3.0

3.3

3.1

3.2

3.0

3.1

3.2

Materials process industries


(refractories); high temperature jigs
and fixtures

Industrial (insulators, sputtering


targets); Net shape parts

not stated

Automotive components; bearings;


wear parts; Net shape parts

Wear parts

650

Mechanical parts (bearings ball


and rollers); High-temperature jigs
and fixtures

Applications(examples)

650

not stated

Hardness
Vickers (GPa, Hv0.5kg)
Vickers (kg/mm2,
Hv0.3kg)
Compressive strength
(MPa)
Flexural strength, 20C
(MPa)
Youngs modulus, 20C
(GPa)
Fracture toughness
(MPam1/2)
Thermal conductivity,
20C
(WmK)
CTE, (10-6 /C) 20C to
1000C

MACgradesaretradenamesofMorganAdvancedCeramics;CERALLOYisatradenameof
CeradyneInc.Dynacer=DynamicCeramicLtd.(1)Lowdensityporousgrade.

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43.14

Zirconium oxide: Zirconia

43.14.1 Typical characteristics


43.14.1.1 General
Pure zirconia undergoes phase transformations with increasing temperature that can result in
significantdimensionalchanges,e.g.about7.5%volumereductionbetween1000Cto1100C.Forthis
reasonitisnotusedcommerciallyasatechnicalceramicinitspureform.
Zirconia usually occurs with hafnium oxide, and this tends to remain in commercial compositions
becauseitisdifficulttoremovetotally.Deliberateadditionsofotheroxides,e.g.magnesiumoxideor
yttria, stabilise the crystal structure of zirconia and so avoid the volumetric changes. This enables a
rangeuseabletechnicalceramicstobeproducedfordifferentapplications.
Commerciallyavailabletypesofzirconiaaregroupedbywhethertheyare:

Fullystabilised:usedlargelyasrefractoriesbecauseoftheirresistancetoattackbymanymolten
metals.

Partiallystabilised:PSZgradeshavecombinedstrengthandtoughness,makingthemsuitable
forengineeringcomponents.

43.14.1.2 PSZ partially-stabilised zirconia


Additions of other oxides can modify and stabilise the crystal structure of zirconia throughout the
intended service temperature range, so limiting the dimensional changes associated with phase
changes.
AthightemperaturesPSZbecomeselectricallyconductive
ThecommerciallyavailablegradesofPSZcanalsobegroupedas:

TZP tetragonal zirconia polycrystal, which have high strengths but moderate usage
temperatures.

TTZ transformation toughened zirconia undergoes a phase change that results in beneficial
compressivestresses,e.g.surfacesundergoingmachiningoratcracktips.

43.14.2 Typical properties


43.14.2.1 PSZ partially-stabilised zirconia
Table 43.14.1 compares the properties of some commerciallyavailable PSZ grades, Ref. [4312], [43
31],[4332].

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Table43.141Technicalceramics:partiallystabilisedzirconiatypicalproperties

Key:

DURA-Z

CoorsTek
YTZP

CEROXIDE

Z900
(MAC Z940R)

94.0

MgO

MgO

Y2O3

3.0% Y2O3

5720
-

5720
-

6020
-

6080
0

5.4% Y2O3
0.25% Al2O3
<1
6000
0

11
78

11.8
77

11.8
77

12.7
81

84

12.5
80

2000

1750

1750

2500

550

620

758

900

1000

200

200

200

210

205

200

8.4

11

11

13

10.0

2.5

2.2

2.2

2.2

2.9

2.9

(2)

10.2

10.3

9.5 (1)

Industrial applications

Industrial applications

Process equipment parts:


(pumps, valves) in
corrosive or abrasive
sectors.

Applications
(examples)

Industrial applications

Grain size (m)


Bulk density (kg/m3)
Porosity apparent (%)
Hardness:
Vickers (GPa, Hv0.5kg)
Rockwell (HR45N)
Compressive strength
(MPa)
Flexural strength, 20C
(MPa)
Youngs modulus, 20C
(GPa)
Fracture toughness
(MPam1/2)
Thermal conductivity
(WmK, 20C)
CTE, (10-6 /C) 20C to
800C

CoorsTek
TTZ

Stabilised

96.5

Industrial applications

Zirconia content (%,


typical) (3)

3.5%
MgO
60
5700
0

10
Process equipment parts:
(pumps, valves) in
corrosive or abrasive
sectors.

Property

Z 500
(MAC 965R)

Examplesofcommerciallyavailablepartiallystabilisedzirconia
grades

10.1

900

MACgradesaretradenamesofMorganAdvancedCeramics;CEROXIDEisatradenameofSCT
SocietedesCeramiquesTechniques,(F);DURAZisatradenameofCoorsTek.(1)20Cto
600C;(2)20Cto1000C;(3)includeshafniumoxidecontent.

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43.15

Structural glass: Glass ceramics

43.15.1 Introduction
43.15.1.1 General characteristics
Glassceramicsareformedfrommoltenglasswhichisthencrystallisedbyheattreatment.Theyconsist
of mixtures of several oxides which form complex, multiphase microstructures. In general the
properties can be tailored by controlling the crystalline structure of the glass matrix. Unlike
conventional sintered ceramics, glass ceramics do not contain porosity which can adversely affect
mechanicalperformance.
Applications for glass ceramics are many and varied; from domestic cookware and appliances, to
industrialusesandstaticanddynamicaerospaceengineeringcomponents,e.g.radomes,engineparts
andmirrorsubstratesforterrestrialorspacetelescopes.
Glassceramicsarestableathightemperatures,havenearzerocoefficientsofthermalexpansionand
areresistanttomanyformsofhightemperaturecorrosionandoxidation.

43.15.1.2 Composition
Themaintypesofglassceramicmaterialsare:

LASlithiumaluminiumsilicate(betaspodumene),whichhasnearzerothermalexpansionup
toabout430C.Whilstthehighsilicacontentgiveslowexpansioncharacteristicsitdoeslower
thestrength.

MASmagnesiumaluminiumsilicate(cordierite),whichingeneral,isbothstrongerandmore
corrosion resistant than LAS. A modified, multiphase version of MAS which contains
aluminiumtitanatehascorrosionresistanceuptoabout1100C.

AS aluminiumsilicate (aluminous keatite), which is produced by leaching the Li from LAS


prior to forming. It also has nearzero thermal expansion up to about 430C. It has been
evaluatedfordynamicpartsinturbineenginesbecauseofitscombinedstrengthandcorrosion
resistance.

43.15.2 Commercially-available glass and glass ceramics


43.15.2.1 Products
Themaincommercialproductscanbesummarisedas:

Zerodur, produced by Schott AG. Zerodur is a wellknown glass ceramic within the space
industryforapplicationssuchasmirrorsubstratesandopticalbenches,[Seealso:43.19].

ULE,producedbyCorningCorp.ULEisatitaniasilicateglassusedwithinthespaceindustry
forapplicationssuchasmirrors.

Macor, which is produced by Corning Corp. but is available throughout Europe from
distributors.

Chemicalmachinablegrades.

GlassbondedMica,alsoknownasaceramoplastic,

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Someexamplesofcommerciallyavailableglassceramicsevaluatedforspaceapplicationsinclude:

HubbleSpaceTelescope:ULEformainmirror;Zerodurforsecondarymirror.

ELTextremelylargetelescopes(Zerodur)

SST(Zerodur)

43.15.2.2 Zerodur
SchottAGproducesZerodur,aglassceramicwithanextremelylowthermalexpansioncoefficient.
Generalcharacteristicsare,Ref.[4335]:

nearzerothermalexpansionwith3Dhomogeneity,

highinternalquality,

goodprocessingbehaviour,

polishabletoahighaccuracy,

easilycoated,

lowHeliumpermeability,

nonporous,

goodchemicalstability.

Zerodurhasbeenevaluatedforapplicationssuchaslightweightmirrorsforastronomicaltelescopes,
bothspacebasedandterrestrial,includingELTprojectsforextremelylargetelescopes(20mto100m).
CommerciallyavailablegradesofZerodurglassesarecategorisedby,Ref.[4335],[4336]:

thermalexpansioncharacteristics,fromClass0to2.

internal quality is determined by the presence and size of inclusions (number and maximum
dimension),striaeandbulkstress(measuredbybirefringence).

Foropticalapplications,theZerodurgradesareknownasstandardorspecial,whereClass0to3
stipulates the internal quality, Ref. [36]. Zerodur M is a variation intended for applications where
processing involves cooling rates more than 0.1K/min, which can affect the CTE values of
components.WhilstZerodurcanbeusedupto600C(mechanicalpartsandwindows),amodified
material known as Zerodur K20 is intended for applications up to 850C. This material has an
expansioncoefficientof1.5106/Katroomtemperatureand2.0106/K(20Cto700C).
Table 43.15.1 gives the basic properties of Zerodur standard grade, Ref. [4335]. Standard grade
ZerodurcoversmaterialsuptoexpansionClass2.

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Table43.151Technicalceramics:Zerodur glass typical properties


Property

Composition
Grain size (m)
Bulk density (kg/m3)
Porosity apparent (%)
Hardness: Knoop (0.1/20)
Tensile strength, MOR (MPa)
Compressive strength, 20C (MPa)
Flexural strength, 20C (MPa)
Youngs modulus, 20C (GPa)
Shear modulus, 20C (GPa)
Fracture toughness (MPam1/2)
Thermal conductivity, 20C (Wm K)
Coefficient of thermal expansion, (106 /K)
Expansion Class, (10-6 /K), 0C to
50C:
Class 2
Class 1
Class 0
Applications(examples)
Key:

SchottAG.commerciallyavailable
Zerodurglassceramic

not stated
2530
0
620
90.3
1.46
0

0 0.10
0 0.05
0 0.02
Astronomy mirrors, inc. GTC Gran Telescopio Canarias (42
inch mirror); ROSAT; SST
solar telescope.

ZerodurisatradenameofSchottAG(D);

43.15.2.3 ULE
CorningInc.ULEultralowexpansionisarangeoftitaniumsilicateglasseswhichhaveparticular
characteristics suitable for applications needing thermomechanical stability combined with optical
performance.ULEhasbeenevaluatedforapplicationssuchaslightweightmirrorsforastronomical
telescopes, both spacebased and terrestrial, and spacecraft applications. Although the basic
characteristicsofthematerialsarethesame,thedifferentcommerciallyavailablegradesofULEare
categorisedby,Ref.[4333]:

thermalexpansioncharacteristics,whichstateguaranteedmaximumlimits(linearcoefficientof
thermalexpansion;deltaCTEvariationsinaxialandradialdirectionsofapart),

opticalretardation,whichismeasuredbybirefringence,

inclusion quality, i.e. the guaranteed maximum numbers of seeds, bubbles and opaque
inclusions.

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ThemaingradesofULEglassesareknownas,Ref.[4333]:

Premium,whichhasthelowestCTEvariations,opticalretardationandinclusions.

Mirror, which exhibits slightly larger CTE variations and birefringence than premium grade,
butthepresenceofinclusionsaredividedintocriticalandnoncriticalzonesandthesizeand
numberpresentaredifferent.

Standard, where the CTE and birefringence values are the same as mirror grade and the
inclusionsarethesameasmirrornoncriticalzone.

Tooling,whichhasnolimitsgivenforCTE,opticalorinclusions.

For EUVL extreme ultraviolet lithography (semiconductor manufacturing) applications, a further


ULEglassgradeisunderdevelopment,i.e.improvedmaterialstraie,whichaffectsurfaceroughness,
andCTEhomogeneity,Ref.[4334].
ULEglassescanbemachinedbymillingandbywaterjet.Componentscanbeassembledusinghigh
temperature joining techniques. Sandwich structures can be manufactured that offer the same
mechanicalandthermoelasticperformanceofmonolithicstructuresarepossible,e.g.forlightweight
mirrorapplications.
Table43.15.2givesthebasicpropertiesofULEglass,Ref.[4333].

Table43.152Technicalceramics:ULE glass typical properties


Property

CorningCorp.commerciallyavailable
ULEglass

Composition
Grain size (m)
Bulk density (kg/m3)
Porosity apparent (%)
Hardness: Knoop (kg/mm2, 200g load)
Tensile strength, MOR (MPa)
Compressive strength, 25C (MPa)
Flexural strength, 25C (MPa)
Youngs modulus, 25C (GPa)
Shear modulus, 25C (GPa)
Fracture toughness (MPam1/2)
Thermal conductivity, 25C (Wm C)
Coefficient of thermal expansion, (10-9 /K)
CTE maximum variation, (10-9 /K) 5C to
35C
Applications(examples)
Key:

titanium silicate
2210
0
460
49.8
69.6
29.0
1.31
0 (0 ppb/C)
30 ( 30 ppb/C)
Astronomy mirrors, e.g. 4.2 m primary
mirror for Lowell Observatory's
Discovery Channel Telescope.

ULEisatradenameofCorningCorporation(USA);

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43.15.2.4 Macor
Macorisamachinableglassceramicwhichcanbemachinedinitsfiredstateusingconventionaltools.
ItscompositionisaproprietaryoxidemixcontainingSi,Mg,Al,K,BandF,Ref.[4312].Someofits
characteristicsinclude:

machinable, stock bar available,

strength, 345 MPa (compressive), 89 MPa (flexural),

modulus, 68 GPa,

high-temperature resistance similar to conventional glass ceramics, e.g. 800C (continuous), 1000C (no
load),

thermal conductivity, typically 1.46 Wm/K,

thermal expansion, typically9.310-6 /C from RT to 1500C,

electrical properties similar to conventional glass ceramics.

If properly baked-out, Macor can meet outgassing requirements.

Someexamplesofaerospaceapplicationsinclude,Ref.[4312]:

ShapedpartsonSpaceShuttleOrbiter,e.g.retainingringsathingepoints,windowsanddoors.

NASAs spaceborne gamma radiation detector uses large pieces of Macor, in which frame
corners are joined by a combination of machined (buttlap) mechanical joints and a sealing
glass.

43.15.2.5 Chemical-machinable grades


Chemicalmachinable grades are photosensitive glasses in their initial state. After sensitising with
lighttocreateapattern,theycanbechemicallymachinedoretchedtoformthecomponent.Thepart
caneitherbeusedasetched,i.e.asglass,orfiredtoconvertittoaglassceramic.Firedglassceramics
can be used where precise tolerances are needed or where a close match to the thermal expansion
characteristicsofmetalsisnecessary,e.g.computerequipment,suchasdiskdriveheadsandprinters.

43.15.2.6 Glass-bonded Mica


Also known as a ceramoplastic, glassbonded mica can be moulded and machined (using carbide
tools) like a plastic but their properties are similar to ceramics. Processing involves heating a green
compact mix of glass and mica until the glass flows, then shaping by a moulding process.
Densification occurs during moulding, so no further firing is necessary after machining. The low
shrinkage of these materials ensures close dimensional tolerances on moulded parts. Thermal
expansion is similar to metals, so enabling mixedmaterial assemblies to be used from cryogenic
temperaturesuptoabout700C, depending on the grade. An example of a commercially-available grade is
MicaTherm HT from Morgan Advanced Ceramics, which can be used continuously up to about 450C, Ref.
[4312]. Applications include domestic, industrial and aerospace components, beyond the capability of polymerbased materials and especially where non-flammability, non-offgassing of toxic fumes and non-outgassing
properties are stipulated.

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43.15.3 Glass ceramics for space applications


Glassceramicsareprocessedasmoltenglasseswithcontrolledcrystallisation.Themainconstituents
aresiliconoxideandaluminabutalsolithiumoxide,zirconiaandtitania.Theprocessingofthemelt
occurs in a similar way as with the processing of glass, however the melt is finally transferred by
temperaturetreatmentintothecrystallineorceramiccondition.Theresultisaglasssimilarproduct
withcontrollablematerialproperties.Atypicalcharacteristicofglassceramicisanegativecoefficient
ofthermalexpansionwithinthetemperaturerangebetween-50Cand300C.
The very low thermal expansion of glass ceramics makes these materials good candidates for the
designofpreciseandhighlydimensionallystableopticalinstrumentsandstructures.
Different types of glass ceramics have been proven in the design and manufacture of optical
instrumentsforspace.Amongstothers,Zerodur,ZerodurM,ULRultralowexpansionglassand
Fused Silica, [See: 43.11], are used for the manufacture of optical mirrors and reflectors but also for
supportstructures,suchasopticalbenches,[See:43.19].
Glassceramicshavealsobeenconsideredasthematrixphaseofcomposites,[See:Chapter53].
Figure 43.15.1 shows the coefficient of thermal expansion of different glass ceramics applied for
opticalinstrumentsinspaceasfunctionoftemperature.

Figure43.151Glassceramics:Coefficientofthermalexpansionwithtemperature
materialsforopticalinstrumentsinspace

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43.15.4 ZERODUR
43.15.4.1 General
Schott AG produce several grades of material. Zerodur glass ceramic is an inorganic, nonporous
material,madebyaprocessofcontrolledvolumecrystallisation.Itcontainsacrystallisedphaseanda
residualglassphasewhichtogetherdeterminethepropertiesofthematerial.Zerodurcontains70to
78weightpercentcrystallinephasewithahighquartzstructure.Thiscrystallinephasehasanegative
linearthermalexpansion,whilstthatoftheglassphaseispositive.Thecrystalshaveanaveragesizeof
about50nm.
Zerodurhasanextremelowcoefficientofthermalexpansion,whichevencanbecomezeroorslightly
negativeinsometemperatureranges.AnotheruniquecharacteristicofZerodurisitsexceptionalgood
homogeneity.Eveninlargematerialblocks,thefluctuationsofmechanicalandthermalpropertiesare
nearly not measurable. A good transparency in the range of about 400nm to 2300nm enables a
verificationoftheinnerqualityofZerodur.Ifneeded,bubblesorinclusionsinZeroduraredetectable.

43.15.4.2 Processing
The Zerodur manufacturing sequence is based on established and proven methods used in the
productionofhighhomogeneityopticalglasses;asshowninFigure43.15.2.

Figure43.152Zerodur:Productionprocessschematic
Themeltiscastintomouldsandinsertedintoannealingovenstocooldowntherawcastingtoroom
temperatureinacontrolledwayforseveralweeks.Intheceramisationprocessthematerialisheated
upagaintoachievecontrollednucleationandgrowthofthecrystalphase;asshowninFigure43.15.3.

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Figure43.153Zerodur:Annealingprocess
The ceramisation process has a large influence on the final homogeneity of CTE within the blank.
Dependingonthesizeofthepart,itcantakeuptoseveralmonths,Ref.[4364].Afterceramisationthe
materialcanbeprocessedtoitsfinalshape.

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43.15.5 ZERODUR: Properties


43.15.5.1 General
AsummaryofengineeringdataforZerodurisgiveninFigure43.15.4,Ref.[4386].

Figure43.154Zerodur:Summaryofengineeringdata
43.15.5.2 Mechanical properties
ThemechanicalpropertiesofZerodurare:

Density: 2.53 g/cm3), Ref. [4387]

Youngs modulus, E : 90 GPa,Ref.[4395]

Poissons ratio, : 0.24, Ref. [4395]

Fracture toughness, KIC : 0.9 MPa m1/2, Ref. [4383], [4385], [4396]

Bending strength and Weibull parameters: Values are dependent on the surface condition, [See: Design].

Flatness: up to /20, Ref.[4387]

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43.15.5.3 Optical properties


TheopticalpropertiesofZerodurare,Ref.[4387]:

Refractive Index, Ref. [4397]:

nd=1.5424(587.6nm).

ng=1.5544(435.8nm).

Transmission;asshowninFigure 43.15.5fora5mmthicksample,Ref.[4387].

Figure43.155Zerodur:Opticaltransmissioncurve
43.15.5.4 Electrical properties
TheelectricalpropertiesofZerodurare,Ref.[4387]:

Dielectric constant:

8.0(1kHz).

7.4(1MHz).

Loss factor tan :

29 10-3 (1kHz).

15 10-3 (1 MHz).

43.15.5.5 Thermal properties


ThethermalpropertiesofZerodurare,Ref.[4387],[4395]:

CTE coefficient of thermal expansion, : 0 0.10 10-6/K, over temperature range 0C to 50C, Ref.
[4387]

Thermal conductivity, : 1.46 W/mK, Ref. [4395]

Specific heat, cp: 0.80 J/gK, Ref. [4395]

Operating temperature, Tmax: up to 600C,Ref.[4387]

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The thermalexpansion characteristicsasa functionof temperature,Ref.[4370], [4374], [4387], [43
102]areshowninFigure43.15.6for0Kto900K,Ref.[4387].
Zerodur is compared with different materials in Figure 43.15.7, Ref. [4374], [43102] and Figure
43.15.8,[4374].

Figure43.156Zerodur:Thermalexpansioncryogenicbehaviour

Figure43.157Zerodur:Coefficientofthermalexpansiondifferentglass
ceramics

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Figure43.158Zerodur:Thermalexpansionofdifferentglassceramics

In Figure 43.15.9, the thermal conductivity is plotted as function of temperature for different glasses, Ref. [4394]. The values of thermal conductivity for Zerodur are located between the two limiting curves in the diagram.
Rangeofthermalconductivityofglasseswithcurvesattemperaturesbetween0Kand500K.Thedata
forZerodur are near to the upper limiting curve high silicate containing glasses, Ref. [4394].

Figure43.159Zerodur:Thermalconductivitycharacteristicsofdifferentglasses

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43.15.6 ZERODUR: Design


43.15.6.1 General
Zerodur is awidelyappliedglassceramicmaterialwithexcellentperformancealsoinspace.Material
properties and design principles for this material arewell documented. Only a rough outline of the
usualdesignprocedureispresentedhere.DetailedinformationisgiveninRef.[4390],[4394],[4396],
[43103],[43104].

43.15.6.2 Design strength


In general, the strength ofglassand glassceramicsis not a material property like Youngsmodulus
becauseitisdependentuponseveralfactors,Ref.[4396]:

microstructureofthesurfacewhichistensionstressedbytheloadapplied,

areaofthesurfaceexposedtotensilestress,

rateofstressincrease,

environmentalconditions

A mechanical failure of glass occurs if two conditions occur together, firstly the presence of tensile
stressatthesurfaceandsecondlythepresenceofaflawintheregionofthetensilestress.Inthecaseof
largeflaws,i.e.morethanabout0.5mmasanorderofmagnitude,orattoohightensilestressesglass
breaksimmediatelyorwithinshortduration.
Ifflawsaresmall,e.g.wellbelow0.5mmorofmicroscopicdimensions,suchflawsgrowslowlyunder
the influence of the tensile stress. If microcracks exceed a critical length their growth accelerates
rapidlyandthematerialfails.Thelargestmicroflawwithinatensilestressloadedareadeterminesthe
strengthofthematerial.
Example: Conservative bending strength values for longterm applications of optical glass and
Zerodur are 8 MPa and 10 MPa respectively. The values are valid for normal surface conditions
withoutscratchesandflaws.

43.15.6.3 Mechanical analysis: Mathematical model


Themathematicalmodelwhichisappliedforthemechanicallayoutofglassceramicsisbasedonthe
Weibulltheory,Ref.[4396].
TheWeibullprobabilityfunctionF(),i.e.probabilityoffailureatbendingstress ,isdefinedby:

F ( ) 1 exp ( / 0 )

[43.151]

wheretheWeibullparametersare:

Characteristic strength, F(0) = 63.21%

Weibull factor, given by the slope of the Weibull line and provides a measure for
the scatter of distribution.

The distribution function is widely used in product lifetime statistics and enables deriving of
predicted failure rates for collectives of identical parts. Based on test results obtained under well
defined conditions, design strengths for loads and conditions defined by special application
requirementscanbecalculated.

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43.15.6.4 Calculation procedure


The calculation procedure described is a short summary of the procedure published in Ref. [4382].
Thenotationusedisadoptedfromthesourcedocument.
Theevaluationofstrengthtestresultsprovides 0 ( S L , 63%,

R ) andforaparticularglasstype

andsurfacecondition.

0 ( S L , 63%, R ) is the characteristic strength for the laboratory test surface area SL and stress
increaserateR.Inthemodelemployedthedesignstrengthdependsontheparameters:
SV

the area of the tensile stress loaded surface

RV

stress increase rate or

tV

the stress load duration time (when constant)

FV

the admissible probability of failure

ThedesignstrengthisderivedfromthelaboratorystrengthbydividingitbyfFOS,thesocalledfactor
ofsafety:

k 0 / f FOS

[43.152]

The factor of safety fFOS is determined as a product of the area factor, probability factor and fatigue
factor.

TheformulaefortheindividualfactorsarederivedonthebasisoftheWeibullmodelusingthelaws
onprobability:

f FOS f A f P f F

[43.153]

where:
fA

area factor

fB

probability factor

ff

fatigue factor

Theareafactor,fA,isdeterminedusingtheexpression:

f A ( S V / S L )1 /

[43.154]

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Eqn. [43.154] assumes constant stress within the loaded area. It is a conservative approach since in
many cases the tensile stress has a maximum value that decreases with distance away from that
maximum.
Foramoreprecisecalculation,Seff,Visused.Thisisobtainedbyweightingthemaximumstresswith
thestressdistributionfunctioninsteadofSV.
Theprobabilityfactor,fp,isdeterminedusingtheexpression:

fp

1 1/
(ln
)
1 FV

[43.155]

Thefatiguefactor,fF,isdeterminedusingthegeneralexpression:

teff ,V
fF
teff , L

1/ n

[43.156]

Where:
t eff,V

effective loading time for the application

t eff,L

effective loading time at laboratory

environmental stress corrosion constant

Ref.[4382]givesamoredetaileddescriptionofparametersteff,Vandteff,L.
Inthespecialcaseofastressloadconstantintime,Eq[43.156]readsexplicitly:

f F (tV f A f P R (n 1) / 0 )1 / n

[43.157]

For application cases with timevarying loads teff,V is calculated instead of tV by using a weighting
functionthatdescribestheloadvariationwithtime.
The stress corrosion constant, n, has been determined for several glass types. If no experimental
resultsareavailable,ncanbeestimatedaccordingtotheexpression:

n 38 2.6

[43.158]

Where:

coefficient of thermal expansion, in units 10-6/K usually at (-30C, +70C)

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ThederivationsoftheformulaeandmoredetailedinformationaboutthecalculationofthefactorsfA,
fPandfFaregiveninRef.[4382].
Table43.15.3showthemeasuredresultsforthecharacteristicbendingstrength,0,Weibullfactorand
stresscorrosionconstant,n,forZerodur,Ref.[4396].
ThetestprocedurewasaccordingtoDIN522921DoubleringmethodR306withastressincreasing
rateof2MPa/s,roomclimateconditionsandatestareaof113mm2.
FailureofprobabilitycurvesofbendingstrengthfordifferentsurfaceconditionsareshowninFigure
43.15.10andFigure43.15.11andasafunctionoftestareainFigure43.15.12,Ref.[4396].
BendingstrengthunderconstantloadisshowninFigure43.15.13,Ref.[4396].

Table43.153Zerodur:Characteristicstrength,Weibullfactorandstress
corrosionfactor

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Figure43.1510Zerodur:Failureprobabilityfortestsurfacesprocessedwith
bondedgritofdifferentsizes

Figure43.1511Zerodur:FailureprobabilityofZerodurfortestsurfaces
processedwithloosegritofdifferentsizes

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The values for the test surface area SL = 113 mm2 are measured by test. Test conditions: Rate of stress
increase 2MPa/s; test surface processed with D 151, air as surrounding medium. The values for the
other test surfaces are calculated.

Figure43.1512Zerodur:Failureprobability,F,asafunctionoftestsurfacearea,
SL

Figure43.1513Zerodur:Bendingstrengthunderconstantload

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43.15.6.5 Fracture toughness


Inthemathematicalmodelpresented,thestrengthofopticalglasswasconsideredfromastatistical
pointofviewbymeasuringthebendingstrengthofsamplesandsubsequentlyestimatingthefailure
probabilities.
Lookingatasingleflawinamaterial,themaximumbendingstrengthdependsonthesizeoftheflaw
andgeometryinthematerial.Forexampleincaseofaflawwithashortdepthinathickplatewith
tensile forces acting normal to the crack plane one can define a stress intensity factor KI by the
expression:

K I 2 0 a

[43.159]

Where:

the nominal stress perpendicular to the stress plane

depth of the flaw.

Aflawresultsinfractureif:

K I K IC

[43.1510]

KICisthecriticalstressintensityfactorforcrackmodeI(tensileforcesnormaltothecrackplane,crack
propagation perpendicular to the forces). KIC is a material constant. For glasses without additional
strengtheningthevalueistypically1.
Table43.15.4providessomefracturetoughnessvaluesforsomeglasses,Ref.[4383],[4385],[4396].

Table43.154Zerodur:Fracturetoughnessofsomeglasses

Foragivennominalstress,theplatewillbreakforacriticaldepthacdeterminedby:

K
ac IC
2 0

[43.1511]

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Example:
ForthecharacteristicstrengthofZerodurofsampleswithD64surfacecondition064MPa,(taken
fromTable43.15.1)andZerodurKIC0.9MPam1/2,thecriticalflawsize,ac,isapproximately49m.
Mostglassesexhibitslowcrackgrowthforastressintensityfactorwellbelowthecriticalvalue.The
mostimportantsubcriticalcrackgrowthoccursinthepresenceofwater(amountslessthen10mgper
m2).Thevelocityofthecrackcanbedescribedusing,Ref.[4384]:

K (a )
da

A I
dt
K
IC

[43.1512]

Where:
a

the depth of the crack,

a constant

stress corrosion constant.

TypicalvaluesforthestresscorrosionconstantofZeroduraregiveninTable43.15.1.
Typically,thesubcriticalcrackgrowcanstartfrom0.25KIC.

43.15.7 ZERODUR: Application examples


Zerodurhasbeenafavouredmaterialformorethan30yearsformirrorsubstratesofterrestrialand
orbitaltelescopes.Owingtotheabilitytoproducelargeamountswithreproduciblequality,itissuited
forfutureELTextremelylargetelescopesprojectsinthe20mto100mclass.

Someothertypicalapplicationsinclude:

Terrestrialastronomicaltelescopes,[See:43.xx].

OpticalbenchforLISApathfindermission,[See:43.xx].

Hubblespacetelescopesecondarymirror.

JWSTJamesWebbspacetelescope(successortoHubble).

MirrorsubstratesandmandrelsforXRaytelescopes.

Opticalelementsforcometprobes.

Ringlasergyroscopes.

Lightweighthoneycombmirrorsupports.

43.15.8 ULE Ultra low expansion titanium-silicate glass


43.15.8.1 General
ULEisproducedbyCorningCorp.CorningCode7972UltraLowExpansionglassisatitaniasilicate
glasswithacompositionof92.5%SiO2and7.5%TiO2.

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Themaincharacteristicscanbesummarisedas:

Verylowthermalexpansion.

Hightemperatureshockresistance.

Highoperatingtemperature.

Such properties have made ULE of interest for use in various applications needing dimensional
precision, e.g. tool reference blocks, components, lasers, solid and lightweight mirror blanks (large
astronomical telescopes; space satellites). Both small and large items can be made successfully, e.g.
fromafewmillimetrestoseveralmetres.

43.15.8.2 Processing
ULE is made by flame hydrolysis. Pure liquid silicon tetrachloride and titanium tetrachloride are
mixedandthevapoursaredeliveredtoafurnace,wheretheyreactchemicallyandtheglassdroplets
depositonaspinningturntable.Theresultingmaterialisatransparentglassceramicwithextremely
lowcoefficientofthermalexpansion(nearzeroatRT)providingdimensionalstability.CTEvariation
withineachbatcharetypically<15ppb/C,radiallyandaxially.

43.15.9 ULE: Properties


43.15.9.1 General
Table43.15.5givesasummaryofengineeringdata,Ref.[43106].

Table43.155ULE:Summaryofengineeringdata

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43.15.9.2 Mechanical properties


ThemechanicalpropertiesofULEare,Ref.[43108]:

Ultimate tensile stress, MOR: 49.8 MPa.

Elastic Modulus, E: 67.6 GPa

Shear modulus, G: 29.0 GPa

Knoop hardness, 200 g load: 460 kg/mm2

Density, : 2.21 g /cm3

Poissons ratio, : 0.17

Softening point (estimated): 1490C

Density (25C): 2.21 g/cm3, Ref.[43107]

43.15.9.3 Optical properties


TheopticalpropertiesofULEare,Ref.[43107]:

Refractive index, Ref. [43107]

nD=1.4828(589nm)

nF=1.4892(486nm)

Transmission; as shown in Figure 43.15.14 for a 10 mm thick sample, Ref. [43107].

Figure43.1514ULE:Transmissioncurve
43.15.9.4 Electrical properties
TheelectricalpropertiesofULEare,Ref.[43107]:

Dielectric constant: 3.99 (100Hz; 25C)

Loss Factor: 0.00005 (100Hz; 25C)

Volume resistivity (D.C.; 200 C;100Hz; R): 1011.6 cm, Ref.[43108]

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43.15.9.5 Thermal properties


ThethermalpropertiesofULEare,Ref.[43107],[43108]:

Coefficient of thermal expansion (5Cto35C):00.1010-9/K

CTE maximumvariation(5Cto35C):3010-9/K

Thermal conductivity, K: 1.31 W/mK, Ref. [43108]

Specific heat, Cp (mean): 767 J/kgK, Ref. [43108]

Thermal diffusity, D: 0.0079 cm2/s, Ref.[43108]

ThethermalexpansioncharacteristicsasafunctionoftemperatureareshowninFigure43.15.15for 100Cto+100C,Ref.[43106].
[Seealso:Figure43.15.7andFigure43.15.8inwhichULEiscomparedwithdifferentmaterials].

Figure43.1515ULE:Thermalexpansioncharacteristics

43.15.10 ULE: Design


The design approach and principles applied for ULE are the same as those described for Zerodur,
[See:Zerodur:Design].

43.15.11 ULE: Application examples


43.15.11.1

General

ULE zeroexpansion glass was originally developed for the space industry to ensure the critical
performanceofopticalsystemsattheextremetemperaturesencounteredduringspacemissions.
ManyofthemajorobservatoriesworldwidehaveprimarymirrorsmadeofULE.
Sometypicalapplicationsinclude:

Ultralowexpansionsubstrates

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Lengthstandards

Lightweighthoneycombmirrormounts

Astronomicaltelescopes

Precisionmeasurementtechnology

Lasercavities

43.15.11.2

Hubble space telescope main mirror

TheHubblemaintelescopemirrorusedULEglassasastructuralmaterial.Toreduceweight,thefront
andbackmirrorplateswerefusedtoahoneycombcoredesign.Thelightweightingtechniquesused
for the Hubble mirror have been extended to other space programs and many groundbased
astronomy applications. The weight of these large mirrors, therefore, is reduced to one eighth the
weightofanequalsizedsolidmirror.

43.15.11.3

Future applications

Currentandfuturespacebasedtelescopesenvisagemirrorsthatarelessthan10percentoftheweight
ofanequalsizedsolidmirror.
ThetechnologyhasbeenadaptedforuseintheGOESWeatherSatellites.

43.16

Speciality materials

43.16.1 Introduction
Althoughclassedastechnicalceramics,thereareawidevarietyofothermaterialsthatofferparticular
characteristicsofpotentialinterestforuseinopticalequipmentandstructures,including:

Beryllia.

Sapphire.

Synthetic diamond.

43.16.2 Beryllia
Berylliumoxide,BeO,isanelectricalinsulatorwithahighthermalconductivityofabout250Wm/K.
Thesepropertieshavemadeitofinterestinthethermalmanagementofelectronics.Itisalsousedin
microwave applications, for items such as windows and radomes. The low thermal neutron
absorptionmakesitusefulinthenuclearindustry.
An example of a commercial >99.5% pure BeO grade is Ceradyne Ceralloy 418, a high thermal
conductivitymaterialforuseinapplicationsneedingheattransfercoupledwithdielectricproperties,
e.g.electronicandmicrowavetubesandIRhighintensityarclamps,Ref.[4338].
Whilstofferingsomeinterestingcharacteristics,theknownhumantoxicityofberylliameansthatvery
specialisedhandlingisneededduringprocessing.Thiswasamajorincentiveforthedevelopmentof
alternativehighthermalconductivityceramics,e.g.aluminiumnitridegrades.

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43.16.3 Sapphire
Synthetic sapphire is an essentially 100% pure, transparent form of alumina consisting of single
crystal (or polycrystalline), hexagonal, alphaalumina. The characteristics vary with respect to the
opticalaxisofthecrystal.
Thegeneralcharacteristicsinclude:

Hardnessapproachingdiamond,e.g.Mohs9,

Strength,~2000MPa(compressive);~900MPa(flexural),

Stiffness,~400GPa,

Fracturetoughness,~2MPam1/2,

Wearresistance(scratchandabrasion),

Wideopticaltransmissionband,e.g.fromUVtonearIR,

Highmeltingtemperature,approximately2050C,

Highelectricalresistance(insulator),

Chemicallyinert,

Goodcorrosionresistance,excepttosomeveryhotcausticcompounds,

Highthermalconductivity,i.e.betterthancopperatcryogenictemperatures.

Numerousgradesofsapphirearecommerciallyavailable,theseareusuallyclassedbytheirintended
application,e.g.formechanicaloropticalapplications(thenbylighttransmissionfrequency).
Sapphire is used for precision mechanical components (bearings, wearparts, coatings) and within
opticalsystems,e.g.lasersystemsandwindowsforimagingsystems.Productformsincludestandard
shapes,suchasrods,tubesandsubstrates,alongwithcustomshapes,e.g.optoelectronicdevicesand
LCDscreens.

43.16.4 Synthetic diamond


43.16.4.1 General characteristics
Thegeneralcharacteristicsofsyntheticindustrialdiamondinclude:

Polycrystallinematerial,

Veryhard(Mohs10),

Highstiffness,

Highthermalconductivity,

LowCTE,

Goodchemicalresistance(acidsandbases),

Electricalinsulator,

Usefulopticalproperties,e.g.transparenttovisible,infraredandUV.

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These combined properties have made synthetic diamond of interest for a wide range of
industrialapplications,e.g.abrasivesandcuttingtoolstocoatingsandshapedpartsforoptical
imagingsystemsand,recently,tweeterconesinloudspeakers,Ref.[439].

Themaintypesofsyntheticdiamondcanbegroupedas:

Abrasives,

Coatings,

Shapedparts.

43.16.4.2 Coatings
Coatings are deposited onto other materials, usually to improve wear and abrasion resistance.
Depending on the proprietary processes used, diamond or DLC diamondlike coatings can be
depositedontopolymers,metals,ceramicsandglass,Ref.[4312].

43.16.4.3 Shaped parts


ProprietaryCVD chemical vapour deposition techniquesare used to createpolycrystalline diamond
shapesuptoafewmmthick,Ref.[439],[4312].
[Seealso:43.17].

43.16.4.4 Developments
Borondopeddiamondhasptypesemiconductorcharacteristics,withpotentialusesintheelectronics
industry,Ref.[4337].
Singlecrystal synthetic diamond, in useable sizes, is under development as a potential replacement
forsiliconinhightemperature,highpowerelectronics,Ref.[4337].

43.17

CVD diamond

43.17.1 Introduction
Since natural diamond flew as a crucial component in one of the Pioneer Venus experimental
payloadsinthemid1970s,diamondtechnologyhasadvancedconsiderably.
UsingproprietaryCVDchemicalvapourdepositiontechniques,thinplatesandshapesinhighpurity
synthetic diamond can now be produced. This has greatly increased the potential applications for
diamond,asmanywereimpracticalduetosizeandshapeusingnaturalmaterial.
Excludingabrasives,someexamplesinclude,Ref.[438],[439],[4310],[4311]:

Optical applications, e.g. windows for missile systems, uses in highpower laser systems,
infraredimagingandprocesscontrolandanalysis,highpowermicrowavesystems.

Thermalmanagementproducts;e.g.substratesforhighpowerelectronicdevices.

Wear parts, e.g. bearings, seals and cutting tools for advanced materials such as MMCs and
CMCs.

Cuttingbladesforprecisionindustrialandmedicaluses.

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Parts for analytical and research equipment, operating at very high pressures (0.5Mbar) and
extremetemperatures(bothhighandcryogenic).

43.17.2 Typical characteristics


Most synthetic CVD diamond is polycrystalline material and many of its final properties are
influenced by the grain structure, e.g. size, orientation, intergranular purity and presence of micro
stresses.Theseareinturnlargelycontrolledbytheprocessconditions.
Althoughsinglecrystalsyntheticdiamondisavailable,thesizesavailablearemuchsmallerandsoof
lessinterestforthermomechanicalengineeringapplications.

Alldiamondproductsareextremelyhardandabrasionresistant,butthebulkmechanical,opticaland
thermalpropertiesofmaterialsfromdifferentsourcescanvarysignificantly.
CommerciallyavailableCVDdiamondmaterialscanbegroupedas,Ref.[438]:

Optical grades: optically transparent with disc thicknesses from 0.3 mm to 1.2 mm and
diameterstypicallyupto120mm,

Mechanicalgrades:darkerinappearancewithbettermechanicalproperties,i.e.strength.Plates
uptotypically140mmdiameter.

Thermalgrades,whichareacompromisebetweenthermalconductivityandcost.

43.17.3 Typical properties


43.17.3.1 General
Table43.17.1givessometypicalpropertiesforacommercialopticalCVDdiamondgrade;Diafilm
OP, produced by Element Six, Ref. [439].

43.17.3.2 Mechanical properties


ThemicrostructureofCVDdiamondislinkedtothesynthesistechniquesandgrowthconditions.In
thicker products it can also vary during the processing; in particular the grain size at the growth
surface is coarser than that at the nucleation surface. Consequently the strength has a strong
dependenceonthethickness,andthecriticalflawsizeisrelatedtothegrainsizeonthefacetested.
Strengthvaluesobtainedfromtestsshowgoodreproducibility.

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Table43.171Technicalceramics:CVDdiamondtypicalproperties
Property

DiafilmOP

Density (kg/m3)
Mechanical:
Hardness (GPa)
Fracture toughness (MPa m1/2)
Youngs modulus (GPa)
Poissons ratio
Tensile strength (MPa):
Nucleation surface
Growth surface
Physical:
Refractive index
Thermal expansion coefficient (ppm/K)
Thermal conductivity (W/m K)
Thermal shock FOM (1) (x 103 W/m)
Specific heat capacity (J/gK)
Dielectric constant, D
Loss tangent (10-6)
Environmental:
Rain impact DTV (m/s)
Sand erosion (mg/kg)
Key:

(1)

3515

Comments

81 18
5.3 to 7.0
1000 to 1100
0.1
800 [11]
400 [23]

2.375
1.0
4.4
1900 to 2200
1100
1000 (approx.)
0.52
5.68 0.15
8 to 20

525
21 6

Fine grain
Coarse grain

at 10m
at 300 K
at 1000 K
at 300K
at 500K
[See: Key]
300K
35 GHz
145 GHz

2 mm drop size
at 100m/s
C300/600 sand

FOM=S(1)k/E;where:=thermalexpansioncoefficient;E=Youngs
modulus;=Poissonsratio;S=strength;k=thermalconductivity

For optical and mechanical grades, the Weibull modulus (for tensile strength), determined from the
results of 3pointbend fracture tests, is given in Table 43.17.2, Ref. [438]. Values corrected for
thicknessvariationarealsoincluded.Ahighvalueindicatesareproduciblestrength.Forcomparison
purposes, typical values for other competitive materials are: sapphire: 2.1, zinc sulphide: 5.4, silicon
carbide:10,Ref.[438].

Table43.172Technicalceramics:CVDdiamondWeibullmodulus
CVDdiamondgrade

Growthsurface
(thicknesscorrected)

Nucleationsurface

Mechanical

9.8 (11.6)

6.5

Optical

11.6 (23.1)

11

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TypicalstiffnessvaluesformaterialgradesatroomtemperatureareshowninTable43.17.3,Ref.[43
8].

Table43.173Technicalceramics:CVDdiamondYoungsmodulus
CVDdiamondgrade

Roomtemperature
Youngsmodulus(GPa)

Mechanical

1166

Optical

1133

Youngs modulus for CVD diamond materials is linked to the occurrence of defects. Materials with
high concentrations of micronsize voids and microcracks give the lowest values, emphasising the
need for rigorous process control. It also shows the importance to designers of accurate property
valuesformaterialgrades,Ref.[438].
The effect of increasing temperature on modulus is moreorless insignificant between room
temperature and 700C; a 5% loss typically. At higher temperatures, the modulus drops as the
diamondbeginstooxidise.

43.17.3.3 Optical properties


[See:ApplicationexamplesforsomethermoopticalpropertiesofCVDdiamond]

43.17.3.4 Electrical properties


[See:ApplicationexamplesforsomedielectricpropertiesofCVDdiamond]

43.17.4 Application examples


43.17.4.1 Pioneer Venus mission
Natural diamond was used for the window of the infrared radiometry experiments carried by the
large probe of Pioneer Venus because of its resistance to the planets extremely hostile atmosphere,
Ref.[438].ThePioneerVenusmultiprobecomprisedofabusthatcarriedonelargeandthreesmall
atmospheric probes. In earlyDecember 1978, all the probes entered the Venus atmosphere at about
11.5 km/s and then decelerated. Parachute deployment occurred at about 47 km altitude. The large
probe,about1.5moveralldiameter,carried7scienceexperiments,withinasealedsphericalpressure
vessel (0.7m diameter), Ref. [4343], including an infrared radiometer to measure distribution of
infraredradiation,whichhadanaturaldiamondwindow,Ref.[438].
Although an example of the use of natural (singlecrystal) diamond, it demonstrates the materials
combined optical and severe environmental resistance in space. After 25+ years of further research
anddevelopment,syntheticpolycrystallinediamondmaterialscannowattainsuchcharacteristics,but
inmuchlarger,useablesizes.

43.17.4.2 Missile infrared imaging windows


One application which exemplifies diamonds combination of optical properties and mechanical
performance in hostile environments is IR imaging windows for airlaunched missiles. These are
domeshaped structures, about 70 mm diameter, forming the nose cone of the missile. As well as

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performingtheiraerodynamicandIRopticalrolesduringtheshort,highvelocitymissileflight,they
resistenvironmentaldegradationformuchlongerperiodswhilemountedonthecarrieraircraft.
Theimportantpropertiesformaterialsinthisroleare:

goodopticaltransmissioncharacteristicsintheimagingsystemwaveband,

highstrengthandstiffness,tosupporthighflightloads(onaircraftandafterdeployed),

preciseshapeandgoodgeometricaltolerances,foraccurateimaging,

goodenvironmentalresistancetotheimpactofrainandsandathighvelocities,

good thermal shock resistance to cope with the high thermal gradients generated during
accelerationandmanoeuvres.

MaterialstraditionallyusedforLWIRlongwavelengthinfrared(8mto14m)detectionsystemsare
ZincSulphideandGermanium.Thesehavepoorerosionresistancetorainandsand,socoatingsare
appliedtoimprovetheirperformance.
AdesigndevelopmentexercisemanufacturedopticalqualityCVDdiamondwindowsintheformof
freestandingdomes,70mmdiameterandover1mmthick.Theradiusofeachsurfacewasmachined
to1m,Ref.[438].
In addition to IR, diamond also has high transparency in other spectral ranges (wavelengths from
0.3m to 3.0m and 7.0m to >500m), enabling it to be used in multispectral windows, e.g.
combinedvisible,IRimagingandlaserrangingsystems.Othermaterialstendtohaveamuchmore
limited transparency range, e.g. 0.4m to 11.5m for ZnS, depending on the grade and 1.8m to
23.0mforGe.
Formissiles,thethermomechanicalcharacteristicsofCVDdiamondaresuperiortoothermaterials.
Diamond has very high thermal conductivity and low thermal expansion, which makes it very
resistant to thermal shock. Thermal shock for CVD diamond can attain a FOM value (103 W/m) of
1000, whereas Ge is 6.1 and ZnS grades are about 2.5. The maximum extended window operating
temperature (in air) for CVD diamond is 1023K, compared with 873K for ZnS. Above these
temperatures,masslossoccursduetooxidation.
TheenvironmentalerosionresistanceofCVDdiamondisconsiderablybetterthanothermaterialsfor
this application. Impacts from highvelocity water drops, simulating operational rain impact, can
seriouslyaffectthemechanicalstrengthofwindowsandreducetheirtransmissioncapabilities,hence
imagingquality.
Repeated sandgrain impact erodes the material surface and degrades the optical transmission
characteristics.ThehardnessandabrasionresistanceofCVDdiamondmakesitthemostresistantof
all the IR materials, including sapphire (used for 3m to 5m spectral band); as shown in Figure
43.17.1,Ref.[438].
Retained transmission for CVD diamond is different depending on which production surface is
exposedtosanderosion,i.e.upperboundisnucleationsurface;lowerboundisgrowthsurface.

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Retained transmission for CVD diamond is different depending on which production surface is exposed to sand
erosion, i.e. upper bound is nucleation surface; lower bound is growth surface.

Figure43.171Technicalceramics:CVDdiamondsanderosion
43.17.4.3 High-power laser systems
A common problem for highpowerlaser windowsmadefrom conventionalmaterials, such as Zinc
Selenide (ZnSe), is thermal distortion of the beam. This is caused by thermallyinduced refractive
indexgradientswherethewindowisheatedbythetransmittedbeam,Ref.[438],[4344].
The characteristics of optical grade CVD diamond (high thermal conductivity, low absorption
coefficient,lowtemperaturecoefficientofrefractiveindex)minimisetheseeffects,enablingitsusein
highpowerCO2laserssystemsforexitwindows,outputcouplers,beamsplittersandlenses,Ref.[43
8],[4344].
Table 43.17.4 compares the typical properties of CVD diamond with ZnSe, materials of interest for
highpowerlasersystems,Ref.[438].

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Table43.174Technicalceramics:CVDdiamondtypicalopticalpropertiesfor
highpowerlasersystems
Property

Thermal conductivity
(W/mK)
Absorption, at 10.6m
(/cm)
dn/dT (10-6 /K)
Key:

CVDdiamond
(opticalgrade)

2000
0.05

(1)

10

ZnSe

17
0.0005

(2)

57

(1)Valuesrangefrom0.1to0.03;
(2)AlthoughthebulkabsorptionofZnSeislower,inpracticetheappliedcoatingsystem
resultsinconsiderablyhighertemperaturerisesinZnSewindowsthanincoated
CVDdiamondundertestcomparableconditions.

43.17.4.4 Microwave windows


Lowdielectriclossmaterialsareusedfortheoutputwindowsofhighpowermicrowavetubes.These
are also structural components as they act as vacuum barriers. All window materials suffer heating
effectstosomeextentintheseapplications,andinpractice,thisiscounteredbycoolingsystems.For
syntheticdiamondwindows,thermalconductivitydecreaseswithincreasingtemperature,whichcan
provoke a thermal runaway effect. However, this can be countered using simple watercooled edge
systems. For severe cases with sapphire windows it can involve the use of expensive cryogenic
coolants,Ref.[438].
AsaresultofdevelopmentworkonimprovingthedielectricpropertiesofCVDdiamond(inthemm
waveband),itisnowusedforGyrotrontubesoperatingfrom70GHzto170GHz,withoutputpowers
inexcessof1MW,Ref.[438].
Fortheapplicationconsidered,theparticulardemandstobemetincluded:

Size: window 100 mm diameter and 1.6mm to 2.3mm thick, depending on microwave
frequency.

Dielectricloss:relativelyuniformoverthewindowareatoavoidhotspots.

Hermeticjoiningofthediamondwindowintoametalflangetosustainhighvacuum.

Modelling of the thermal performance of CVD diamond windows transversed by a 1.2 MW beam
showedthatformaterialswithadielectriclossvalueoftan<104,thecentraltemperaturerisewas
lessthan240Cwithasimplewatercoolededge,whichistolerablefordiamond.
Table43.17.5givessometypicalpropertiesofcommerciallyavailableDiafilmdielectricgradeCVD
diamond,Ref.[438].
For highpower Gyrotron tube applications, the predicted temperature rise in dielectric grade
materials is under 15C. This means that CVD diamond dielectric grades can perform above 1MW,
andalsoincontinuouswavemodeatpowersaround0.5MWwithouttheneedforcryocooling.

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Table43.175Technicalceramics:CVDdiamondtypicaldielectricproperties
forhighpowermicrowavesystems
Property(2)

Loss tangent, tan


( 10-6 )
Equivalent
absorption, (/cm)
Relative permittivity,
r
Key:

Diafilm(1)

Comments

(dielectricgrade)(3)

20 to 50
0.0014 to 0.0035
5.68

Typical values, maximum value


100 10-6
Typical values, maximum value
0.007/cm
Typical value

(1)DiafilmisatradenameofElementSix(UK,NL);
(2)Datameasuredatfrequency=145GHz(wavelength,=2.1mm);
(3)availablesizes:upto120mmdiameterand2.25mmthick.

43.17.4.5 Cutting blades


The ability to retain a sharp edge during repeated use, coupled with hardness and wearresistant
properties has made CVD diamond attractive for precision cutting blades for both industrial and
medicaluses,including,Ref.[438]:

fibreopticassembly,whereadiamondcuttingbladesproducecleancleavageofopticalgrade
glassfilaments.

medicalapplications,e.g.

Ultrasharpdiamondscalpelsforopthalmicsurgery.

Laserscalpels,wherethediamondbladeiscombinedwithalasercauterisingsystem.

Ultramicrotamy for the preparation of very thin, typically 100nm thick, slices of tissue for clinical
analysis.

43.18

Cesic: NIRSpec optical bench

43.18.1 Introduction
Under ESA contract, Alcatel Space (F) and ECM (D), designed, manufactured and tested a flight
representativeopticalbenchmadeofCesic.ThiswasanapplicationfortheNIRSpecinstrumenton
theJamesWebSpaceTelescope.
Theopticalbenchwassuccessfullysubmittedtointensiveshakervibrationtests,upto80g,without
problemandshowedveryhighstabilitywhentesteddowntoatemperatureof30K.

43.18.2 Material characteristics


43.18.2.1 Ceramics
Ceramicmaterialsareofinterestforspaceinstrumentsbecauseoftheircharacteristics,including:

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High specific stiffness and large mechanical dimensional stability (no residual deformation), and thermal
and thermoelasticperformances.

High thermal conductivity, high /a ratio enabling through thermal conduction, good thermo-elastic
behaviour, homogeneity, low coefficient of thermalexpansionandremarkablecryogenicbehaviour.

[See:43.1]

43.18.2.2 Cesic
From amongst the many different types of ceramic materials, Cesic from ECM in Germany was
selectedbyAlcatelSpaceasthebestcandidateforuseinthedevelopmentofstructuresandmirrorsof
future space instruments. Knowledge of the material itself, along with all the associated processes,
enabledCesictobeconsideredasamaturetechnology.
CesicisaceramicmadeofSiC,SiandC.Itismadebythereaction,athightemperaturebetweenaC
Cgreenshapeandliquidsilicon,Ref.[4357].

[Seealso:43.12]

43.18.3 Development of optical bench


43.18.3.1 NIRSpec
During the NIRSpec development phase for the JWST James Web Space Telescope project, a large
designdevelopmentprogrammewasinitiatedunderESAcontract,withAlcatelSpace,inFrance,and
ECM,inGermany.

43.18.3.2 Development programme


Theaimofthedevelopmentsprogrammewasto:

Manufacture and test an optical bench representative of NIRspec in dimensions, shape and
designinorderto:

demonstratethefeasibilityoftheconcept,

validatetheentiremanufacturingprocesses.

Based on an elementary characterisation of Cesic material, to demonstrate that the material is


homogenous enough to avoid any unwanted distortion at cryogenic temperatures.

Perform vibration tests to demonstrate that:

Theequippedbenchcansupportthemechanicallaunchenvironmentwithoutdamage.

Validateloadsintroducedbythebenchtoequipmentduetoitsdampingbehaviour.

Verify bench stability under tests down to the cryogenic working temperature of 30 K.

43.18.3.3 Demonstrator structure


Anopticalstructure,fullyrepresentativeoftheNIRspecopticalbench,exceptforsize,wasdesigned,
dimensioned and manufactured successfully. The bench produced was 1045mm 600mm 100mm
andthemasswas23kg.

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The designand size constraints usedfor the benchwere the optical and launch loads, butalso took
intoaccounttheflexibiltyofmanufacturingpartswithCesic;notablybyproducingahalfclosedback
design to maximise stiffness, Ishaped stiffeners, thin ribs to minimise mass, CC blocks at interface
junctionsandholescutusingEDMelectrodischargemachiningtechniques.
Figure43.18.1showsthemainfeaturesofthedemonstratoropticalbenchproduced.

I-shaped
stiffeners to
optimise specific
stiffness
Seconda ry ribs and hole s for mirr or
sup port I/F and fixing by bo lts

Figure43.181NIRSpecopticalbenchdevelopment:Cesic
structure

ceramic demonstrator

43.18.3.4 Mechanical testing


Tosupportthedesignandvalidatethepropersizing,representativetechnologysamplesweretested
uptoultimateloads;asshowninFigure43.18.2.
Thetestsresultsconfirmedthestrengthofthejointareaandshowednolossofstiffnessandstrength.
The test results also showed good correlation with the FEM finiteelement model, including failure
loads.
Representativefullyinstrumentedbenchcellshavealsobeentesteduptoultimateload.
Figure 43.18.3 show the test setup. These tests established a large safety factor margin for the
designedflightbench:factorofsafety3.

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Machined surfaces
with close parallel
tolerances

Joint line

Articulated
load points

Figure43.182NIRSpecopticalbenchdevelopment:TestsetupandIbeam
samplewithjointline

Figure43.183NIRSpecopticalbenchdevelopment:Testsetupforinstrumented
benchcells
43.18.3.5 Vibration testing
Theentirebenchwastestedundervibration.Theobjectivesoftheopticalbenchvibrationtestswere
to:

Identify the dynamics behaviour of such representative flight bench, e.g. amplification,
dampingcoefficient.

Validatethestiffnessofthebench.

Validatethestrengthandidentifytheeventualmarginfortheallowablestrengthnecessaryfor
thesizingofafutureNIRspecflightbench.

To establish the strength and margins, the bench underwent vibration testing up to the maximum
sinuslevelpossiblebytheshaker,i.e.morethan80gatshakerlevel.Thevibrationlevelsimposedon

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the test bed exceed the qualification loads experienced by a fullsized flight bench, the bench was
thereforequalifiedforflight.
Figure43.18.4showsthebenchinstalledontheshaker.

Figure43.184NIRSpecopticalbenchdevelopment:Testsetupforshaker
vibrationtests

TheFEMpredictionwascorroboratedbythetestresults,whichconfirmedthematerialpropertiesand
alsotheabilitytopredictstiffness,stressandstrengthbehaviour.
The bench eigenfrequency is above 500Hz and the amplification factor, measured during OBB sine
test,islessthanQ=30,solimitingloadsinducedoncriticalequipmentundervibrationandnotching.

43.18.3.6 Cryogenic testing


Thestabilityoftheopticalbenchwasdemonstratedbytestingatcryogenictemperatures;from300K
down to 30K. The test was performed in CSL (Belgium) in focal V chamber. The bench was cooled
through cryohelium panels by a radiative and conductive link. Figure 43.18.5 shows the bench
installedinthecryogenictestchamber.

Invar rule
Extension
bench at 90
BENCH
Thermal
sensors
Cryo panels
Thermal
straps

Figure43.185NIRSpecopticalbenchdevelopment:Testsetupforcryogenic
temperaturetest
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During the test, the inplane contraction and the outofplane stability was measured by a speckle
holographic interferometric method. This technique provides an accuracy of around 1m on the
wholecyclewitharesolutionof0.1m.ThemeasurementwasperformedbyHOLO3.
Duringthecryogenictest,allthecriteriaweremetsuccessfully,i.e.:

Temperatureoflessthan30KwasreachedbyOBB.

Thermalcontractionwasaspredictedfrommeasurementofsamples:

contractionwashomogeneousonthewholebenchsurface;asshowninFigure43.18.6.

benchdeformationwaszerofrom100Kto30K;asshowninFigure43.18.7,whereallthe
curves from different positions are combined to also show that the contraction was
homogeneousoverthesurface.

Outofplane deformation was quasizero between 293K and 30K; as shown in Figure 43.18.8.
Thisenablesgoodopticalalignmenttobemaintainedduringcooldownfrom300Kto40K.No
hysteresiswasobservedduringtheentirethermalcycle.

The overall results of the cryo testing demonstrated that the bench structure made of Cesic was
highly stable. It was concluded that Cesic is a suitable material for making dimensionallystable
structuresoperatingundercryogenicconditions.

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0.25 m deformation due


to thermocouples bonded
onto back face
Invar ruler

Holographic measurement between 30K and 90K

+100

+50

-50

-100

Displacement dx between 35K and 291K

Figure43.186NIRSpecopticalbenchdevelopment:Thermalcontractionunder
cryogenictest

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Linear displacement dx/x in x-direction

Optical bench mean temperature, K

Figure43.187NIRSpecopticalbenchdevelopment:Lineardisplacementunder
cryogenictest

Figure43.188NIRSpecopticalbenchdevelopment:Outofplanedisplacement
undercryogenictest

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43.18.4 Conclusions
The large development study, performed jointly by Alcatel Space and ECM and supported by ESA,
demonstratedthatCesicisamaturetechnologywhichcanbeconsideredforapplicationsneeding:

Structural optimisedshaped components, e.g. mechanical performance combined with the


processingflexibilitytoproducemassefficientcomponents,i.e.veryhighEI/Mratio,

Mechanicalproperties,e.g.highstrength,insensitivetofatigue,goodsurfacefinishes,atjoints
andinterfaces,boltedjointsunderhighloads.

Processing using an established material production route, along with accurate machining by
EDMtoprovideprecisioninterfaces.

Mirrormanufacturingcapability,i.e.abletoproducelargelightweightandstiffmirrors;mirror
withintegratedfilteringMFD.

Highstability performance under cryogenic temperatures for dimensionally stable structures,


e.g.opticalandtelescopesupports.

Costandtimeefficientmanufacturing.

Potential to evolve further, e.g. manufacturing of more complex shapes and structures;
enhancedproperties.

43.19

Zerodur: Applications case study

43.19.1 Introduction
For over 30 years, Zerodur has been a material favoured for mirror substrates of terrestrial and
orbitaltelescopes.Morethan200astronomicalmirrorblankswithdiametersbetween1mand2mhave
beenproduced,Ref.[4368].
The ability to produce large amounts with reproducible quality makes it suitable for future ELT
extremelylargetelescopesinthe20mto100mclass.
Modern fabrication technologies enable the production of structures with more than 65% weight
reduction.Owingtoitsgoodhomogeneityofcoefficientofthermalexpansion,Zerodurisalsousedas
a mandrel material for shaping mirror shells, such as those envisaged in future Xray telescope
projects
The material has been used in a large number of optical instruments for different space missions,
including the secondary mirror of the Hubble Space Telescope. It is also intended to be used in its
successor;JWSTJamesWebbSpaceTelescope.
Somefurtherapplicationsforspaceinclude:

MirrorsubstratesforXraytelescopes.

Opticalelementsforcometprobes.

Ringlasergyroscopes.

Lightweighthoneycombmirrorsupports.

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43.19.2 Terrestrial mirrors


Ageneraloverviewon100mirrortelescopesmadeofZerodurisgiveninRef.[4368].
Table43.19.1givesanoverviewoflargeterrestrialmirrorblankprojects,Ref.[4368].

Table43.191Zerodur:Overviewofterrestrialastronomicaltelescopemirrors

43.19.3 Optical bench


Figure 43.19.1 shows a breadboard of an optical bench made of Zerodur for the LISA Pathfinder
Mission.Zerodurwasselectedasastructuralmaterialbecauseitsthermallystablebehaviourmetthe
extremerequirementstodetectgravitationalwaves.

Figure43.191Zerodur:OpticalbenchforLISApathfindermission

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43.20

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TechnologiesII(2005)p.241251

[4370]

O.Lindig&WPannhorst
ThermalexpansionandlengthstabilityofZERODURindependence
ontemperatureandtime
AppliedOptics,Vol.24,No.20,p.23303334,1985

428

ECSSEHB3220Part4A
20March2011
[4371]

F.BayerHelmsetal
LngenstabilittbeiRaumtemperaturvonProbenderGlaskeramik
ZERODUR
Metrologia21,p.4957,1985

[4372]

R.Haugetal
LengthvariationinZERODURMinthetemperaturerangefrom60C
to+100C
AppliedOptics,Vol.28,No.19,1989

[4373]

R.B.Robertsetal
ThermalpropertiesofZERODURatlowtemperaturesCryogenics22,
p.566,November1982

[4374]

J.H.Burgeetal
ThermalexpansionofBorosilicateglass,ZERODUR,ZERODURM,
andunceramizedZERODURatlowtemperatures
AppliedOptics,Vol.38,p.7161,1999

[4375]

J.W.Baer&W.P.Lotz
Figuretestingof300mmZERODURmirrorsatcryogenic
temperatures
ProceedingsofSPIECryogenicOpticalSystemsandInstrumentsIX,Vol.
4822,2002

[4376]

SchottAG:ZERODURglassceramic
Catalogue10162e09043.0

[4377]

K.SchillingSCHOTTInternalreport303/91Mainz1991

[4378]

H.Richter&G.Kleer:FraunhoferInstitutfrWerkstoffmechanik,Freiburg
(D)
ReportV24/83(1983)

[4379]

M.J.Viens
NASATechnicalmemorandum4185(1990)

[4380]

F.Kerkhofetal:
Glastech.Berichte54(1981)No.8p.265to277

[4381]

G.Exner&O.Lindig
GlastechBerichte55(1982)No.5p.107to117

[4382]

G.Exner,SchottGlaswerke,Mainz(D)
GlastechBerichte56(1983)Nr.11,p.299312

[4383]

H.Bach&N.Neuroth(Editors)
Thepropertiesofopticalglass
SpringerVerlag1998

[4384]

S.M.Wiederhorn,L.H.Bolz
Stresscorrosionandstaticfatigueofglass
J.Am.Ceram.Soc.53,543548(1970)

429

ECSSEHB3220Part4A
20March2011
[4385]

M.J.Viens
FracturetoughnessandcrackgrowthparametersofZERODUR
NASATechnicalMemorandumA969903(1990)

[4386]

INSACOInc.(USA)http://www.insaco.com/MatPages/zerodur.asp

[4387]

PraezisionsGlas&OptikGmbH,Iserlohn(D)
http://www.pgoonline.com/intl/katalog/zerodur.html

[4388]

SCHOTTAG,Mainz(D):Datasheetfromwebsite
http://www.schott.com/optics_devices/english/
2TIE25Striaeinopticalglass

[4389]

SCHOTTAG,Mainz(D):Datasheet
2TIE26Homogeneityofopticalglass

[4390]

SCHOTTAG,Mainz(D):Datasheet
2TIE27Stressinopticalglass

[4391]

SCHOTTAG,Mainz(D):Datasheet
2TIE28Bubblesandinclusionsinopticalglass

[4392]

SCHOTTAG,Mainz(D):Datasheet
2TIE29Refractiveindexanddispersion

[4393]

SCHOTTAG,Mainz(D):Datasheet
2TIE30Chemicalpropertiesofopticalglass

[4394]

SCHOTTAG,Mainz(D):Datasheet
2TIE31Mechanicalandthermalpropertiesofopticalglass

[4395]

SCHOTTAG,Mainz(D):Datasheet
2TIE32Thermalloadsonopticalglass

[4396]

SCHOTTAG,Mainz(D):Datasheet
2TIE33DesignstrengthofopticalglassandZerodur

[4397]

SCHOTTAG,Mainz(D):Datasheet
2TIE34RoHSfrequentlyaskedquestionsJuly2005

[4398]

SCHOTTAG,Mainz(D):Datasheet
2TIE34RoHSAnnexpresentstatus

[4399]

SCHOTTAG,Mainz(D):Datasheet
2TIE34RoHSHazardoussubstancesinopticalglass

[43100] SCHOTTAG,Mainz(D):Data
2TIE35Transmittanceofopticalglass
[43101] SCHOTTAG,Mainz(D):Datasheet
2TIE36Fluorescenceofopticalglass

430

ECSSEHB3220Part4A
20March2011
[43102] SCHOTTAG,Mainz(D):Datasheet
2TIE37ThermalexpansionofZERODUR
[43103] SCHOTTAG,Mainz(D):Datasheet
2TIE38LightweightingofZERODUR
[43104] SCHOTTAG,Mainz(D):Datasheet
2TNE03Materialsafetydatasheetabbreviationexplanation
[43105] SCHOTTAG,Mainz(D):Datasheet
2TNE04Testreportfordeliverylots
[43106] INSACOInc.(USA)
http://www.insaco.com/MatPages/corning_ule_glass.asp
[43107] PraezisionsGlas&OptikGmbH,Iserlohn(D)
http://www.pgoonline.com/intl/katalog/ule.html
[43108] CorningCorp.(USA):SemiconductorOptics
http://www.corning.com/semiconductoroptics/technical_information/
<SEARCHforULE>
CorningInternationalEurope,Wiesbaden(D);email
cieurope@corning.com
[43109] A.A.vanVeggel:EindhovenTechnicalUniversity/TNO(NL)
ExperimentalEvaluationoftheStabilityandMechanicalBehaviourof
ContactsinSiliconCarbidefortheDesignoftheBasicAngleMonitoring
SystemofGAIA
ProceedingsofEuropeanConferenceonSpacecraftstructures,Materials
andMechanicalTestingESAESTECNoordwijk(NL)1012May,2005.
ESASP581(August2005)
[43110] BoostecS.A.website:http://www.boostec.com/index.htm
Materialcharacteristics:
http://www.boostec.com/SiCTypicalCharacteristics.pdf
Otherhighprecisioncomponents:http://www.boostec.com/real.htm
[43111] S.Williams&P.Deny:CoorsTekInc(USA)/BoostecIndustries(F),
OverviewoftheproductionofsinteredSiCopticsandopticalsub
assemblies,
OpticalMaterialsAndStructuresTechnologiesII(OEI402),
SPIEOpticsandPhotonics2005,SanDiego,CA
[43112] G.vanPapendrecht
OutgassingtestonSiliconcarbidesamples
MaterialsReportNumber:3959,QMCreportnumber:QMC2004/099,21
June2004,MaterialsPhysicsandChemistrySection,Materialsand
ProcessesDivision,ESTEC
[43113] CastelD.(Astrium),DenauxD.(Astrium),BourgoinM.(Boostec),Mercier
K.(CNESToulouse)
NewTechnologyforManufacturingVeryLargeSiCMirror

431

ECSSEHB3220Part4A
20March2011
EuropeanConferenceonSpacecraftStructures,MaterialsandMechanical
Testing,Toulouse,(France),1113December2002
[43114] OpticalBenchBreadboard,
NearInfraredSpectrographforJWST,
FinalReport,Doc.No.:NGSTASDTR007,dated18.3.2004
[43115] SI01NIRSPECDesignReporttoESTEC,
Doc.No.NIRSASDRP0001,dated01.10.2004

43.20.2 Sources
Dataareforillustrativepurposesonlyandcannotbeusedfordesign.
All data presented and cited within the text are summarised from informationprovided directly by
materialsuppliersorobtainedfromtheirwebsites(toend2005).

43.20.3 ECSS documents


[See:ECSSwebsite]

ECSSQ7071
ECSSQST7001
ECSSQST7002

Datafortheselectionofspacematerials
andprocesses,previouslyESAPSS01701.
Cleanlinessandcontaminationcontrol
Thermalvacuumoutgassingtestforthe
screeningofspacematerials;previously
ESAPSS01702

43.20.4 Other standards


ISOstandards

EN606721
EN606722
EN606722

Fineceramics(advancedceramics,advanced
technicalceramics),[See:43.3]

CeramicandglassinsulatingmaterialsPart1:
Definitionsandclassification
CeramicandglassinsulatingmaterialsPart2:
Methodsoftest
CeramicandglassinsulatingmaterialsPart3:
Specificationforindividualmaterials

[Seealso:81.9forCENceramicrelatedstandards]

432

ECSSEHB3220Part4A
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44
Magnesium alloys and their composites
44.1

Introduction

44.1.1

General

The main magnesium alloys are listed, together with their chemical compositions and typical
mechanicalproperties.
Bothdiscontinuouslyreinforcedandcontinuousfibrereinforcedcompositesaredescribed,alongwith
potentialapplicationsforboth.

44.1.2

Features

Thebasicfeaturesofmagnesiumalloysinclude:

Low density (1740 kg/m3), which makes Mg attractive.

Low thermal stability, giving limitations in terms of thermal performance (usually to temperatures below
100C, but new alloys extend range towards 200C).

High damping capacity, good resistance to vibration fatigue.

High CTE, e.g. 27 to 28 10-6 /K between 20C and 300C.

Processing, where the c.p.h. crystal structure of most magnesium alloys meansthatextrudedandsheet
products are more difficult to manufacture than aluminium alloys, hence more costly. Good
fluidityofmagnesiumcastingalloysmeansthatawiderangeofnearnetshapecomponentsare
available.

[Seealso:ECSSQ7071]

44.1.3

Alloy classification

Table 44.1.1 provides the ASTM system of alloy and temper designations for magnesium alloys.
Conventionalalloyspecifications,plussupplierproductcodes,areprovidedinRef.[446],[4420].

433

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Table44.11Magnesiumalloys:ASTMdesignationsystemalloysandtempers
Firstpart
Indicates the two
principal alloying
elements
Consists of two
code letters
representing the
two main alloying
elements
arranged in order
of decreasing
percentage (or
alphabetically if
percentages
equal)

A - aluminium
B - bismuth
C - copper
D - cadmium
E - rare earth
F - iron
G - magnesium
H - thorium
J - strontium
K - zirconium
L - lithium
M - manganese
N - nickel
P - lead
Q - silver
R - chromium
S - silicon
T - tin
V - gadolinium
W - yttrium
X - calcium
Y - antimony
Z - zinc

Secondpart
Indicates the
amounts of the two
principal alloying
element
Consists of two
numbers
corresponding to
rounded percentages
of the two main
alloying elements,
arranged in same
order as alloy codes in
first part

Thirdpart

Fourthpart

Indicates minor
variations to the
basic designation

Indicates condition
(temper)

Consists of a letter
of the alphabet
assigned in order
as compositions
become standard

Consists of a letter followed


by a number (separated
from the third part of the
designation by a hyphen)

F-as fabricated
O-annealed, recrystallised
(wrought products only)
H-strain hardened
H11 (slight) to H18 (fully) strain hardened
H21 to H28 - strain
hardened and partially
annealed (H21 softest)
H31 to H38 - strain
hardened and stabilised to
prevent age softening
T1- cooled and naturally
aged
Whole numbers

Letters of alphabet
except I and O

T3- solution heat treated


and cold worked
T4- solution heat- treated
T5- cooled and artificially
aged
T6-solution heat-treated
and artificially aged
T7- solution heat treated
and stabilised
T8- solution h.t. cold
worked and artificially
aged
T9- solution h.t. artificially
aged and cold worked
T10- cooled artificially aged
and cold worked

434

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44.1.4

Environmental aspects

44.1.4.1

General

Magnesium is resistant to attack by alkalis but is attacked by most acids. Similarly, magnesium is
attackedbycommonacidicsaltssuchaschloridesolutionsfoundintheformofseawater.Therefore,
unlessamagnesiumcomponentistofunctioninaninnocuousenvironment,itshouldnotbeusedin
servicewithoutsomeformofprotectivetreatment.
Magnesium alloys are not prone to intergranular attack since the grain boundaries are cathodic
compared with the actual grains and would therefore be cathodically protected if exposed to a
corrosiveenvironment.
Inaddition,mostmagnesiumalloys,withtheexceptionofthemagnesiumaluminiumalloys,arenot
susceptible to stress corrosion cracking under normal conditions and at stresses up to 0.2% Proof
Stressvalues,Ref.[449].

[Seealso:ECSSQST7036]

Cathodicimpurities,e.g.iron,nickel,copper,canhaveasignificanteffectonthecorrosionbehaviour
of unprotected magnesium alloys and are therefore controlled to low levels in alloys specified for
aerospaceanddefenceapplications.
Conversely,surfacecontamination,forexamplebyminutecathodicparticlesresultingfromabrasive
blastingwithcastironorsteelshot,mayresultinhighcorrosionrates.
Galvaniccorrosioncanalsoariseatdissimilarmetalattachments,suchasnuts,boltsandrivets,unless
thenecessaryprecautionsaretaken.

44.1.4.2

Protection systems

A number of well proven protective coating systems and techniques are available and these are
generally based on anodising or a chemical conversion treatment (usually chromating) followed by
painting, Ref. [449]. However, chromating is being phased out due to health and safety legislation
concerning chromate baths and a number of new protective systems have been developed, such as
Tagnite,KeroniteandOxsilan.Thedesignerthereforeneedstoconsultthematerial,component
supplierorspecialisttreatmentcompaniesatanearlystage.

44.1.5

Machining

Theflammabilityoffinelydividedmagnesiumintheformofmachiningswarforgrindingdustmeans
thatduecaremustbeexercisedwhenmachiningmagnesiumalloys.
Likewise, there is potential for hydrogen generation should water based cutting fluids be used.
However, magnesium alloys show very good free cutting and may be machined faster, without
cutting fluids and at lower power than aluminium alloys, allowing complex shapes with close
tolerancestobeeasilymanufactured.
Guidanceonmachiningparametersandtherelevantsafetyproceduresarewelldocumented,Ref.[44
10],althoughthiswillnormallybetheresponsibilityofthecomponentsupplier.

435

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44.1.6

MMC - metal matrix composites

Considerable activity on discontinuously reinforced (particulate) magnesiumbased MMCs occurred


duringthe1980sand1990sandsomematerialswerecommercialised,[Seealso:44.3].However,the
costofproductionofthesematerialshasresultedintheirwithdrawal,althoughproductioncouldbe
reinstatedifthedemandjustifiesthehighsetupcosts.
WorkcontinuesoncontinuousfibrereinforcedMMCs,mainlyintheUSAwheremuchoftheactivity
is restricted, with the primary interest being on low CTE materials for electronics packaging or
substratesforspacemirrors.
AnindicationofthetechnicaldevelopmentandcommercialavailabilityofMMCsisprovidedonthe
websiteoftheMMCAssessproject.

44.1.7

Material availability

44.1.7.1

General

ManyoftheestablishedmagnesiumalloyscontainedThoriumasamajoralloyingelement.Owingto
concerns over residual radioactivity, these alloys have been withdrawn from regular commercial
supplyandarethereforenotincludedinthishandbook.
Also,whilstsuperlightmagnesiumlithiumalloysweredevelopedinthe1960s(andusedintheUS
Saturn programme)and the higherlithiumalloyshave a b.c.c.structure which is moreamenable to
extrusionorrolling,difficultiesinthefoundryproceduresandconcernsovercorrosionresistancein
aqueousenvironmentshavelimitedtheuseofthesealloys.FurtherworkiscontinuinginGermany,
Ref.[4413],andJapanbutnonewalloyshaveasyetbeenregisteredcommercially.

44.1.7.2

Sources

Table44.1.2liststhemajorcommercialsourcesofmagnesiumalloys.Alloysandproductformsvary
betweensuppliers,Ref.[446].
NOTE

Further information on magnesium suppliers is available from:


International Magnesium Association (www.intlmag.org) and
DMTC Israeli Consortium for the Development of Magnesium
(www.dmtc.org.il).

Table44.12Magnesiumalloys:Sourcesexamples
Supplier

Website

Alubin (Israel)
AMTS, Wrought Product
Division (Israel) (1)
Dead Sea Magnesium (Israel)
Hydro Magnesium (Norway)
Magnesium Elektron (UK)
Otto Fuchs (D)
Timminco (Canada)

www.alubin.com
www.magnesiumtechnologies.com
www.dsmag.co.il
www.hydromagnesium.com
www.magnesium-elektron.com
www.otto-fuchs.com
www.timminco.com

Key:

(1)LinkswithChemetallGmbH(D)forsurfacetreatment.

436

ECSSEHB3220Part4A
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44.1.8

Future developments

Muchofthedevelopmentactivityonmagnesiumalloysinrecentyearshascentredonapplicationsin
the automotive industry, where weight reduction has been seen as a means to improving fuel
efficiency.Becauseofthegoodcastabilityandeconomicsofhighvolumeprocesses,thethrustofthis
has been on alloys for pressure diecasting. The drawbacks with existing casting alloys have been
twofold:poorhightemperaturepropertiesandlowroomtemperatureductility.

Alloys have now been introduced with improved properties both at room temperature and in
elevatedtemperaturecreepresistance.
Whilst diecastings may not have been normally considered for aerospace applications, the
improvementsinprocesstechnologyhaveresultedintheavailabilityofhighqualitycomponentswith
closetolerancenearnetshape.Also,whilsthighinitialtoolingcostsareinvolved,theoverallcostof
thecomponentscanstillbecompetitivewithalternativemanufacturingroutesevenatlowvolumes,
Ref.[4415].Someofthenewdiecastingalloysarethereforegiven,[See:44.2].
There has also been much activity in attempts to improve the economics of production of wrought
magnesiumproductswhichhavetraditionallybeenmorecostlythanaluminiumproductsduetothe
lowerprocessingspeedsofmagnesiumalloys.
Magnesium sheet products produced by twinroll casting are becoming available and work is also
progressingonimprovedextrusionprocesses.
A new high strength extruded alloy, Elektron 675, has recently been announced by Magnesium
Elektronand,whilstthisisstillundergoingfinaldevelopment,itstensilepropertiesat200Carebetter
than2024or7075aluminiumalloyswhichmakesitofpotentialinterestforaerospaceapplications.
FurtherworkcontinuesatvariousUniversitiesandresearchcentresonalloysforhighertemperature
applications, superlight MgLi alloys and on Mgbased MMCs. However, the economics of
productionmeanthatfewofthesearelikelytoreachcommercialavailability.

44.2

Magnesium alloys

44.2.1

Chemical composition

Table 44.2.1 indicates the nominal chemical compositions of many magnesium alloys. The
compositions are classed by the method used for processing and the alloys are listed using their
ASTMdesignationsandUNSnumberswhereregistered,Ref.[4420],[4421],covering:

Sand and permanent mould castings

Die castings

Wrought products

[Seealso:Table44.1.1forASTMdesignationsystem]

Someproprietaryalloysarealsoincludedtogetherwithsomerecentalloys,Ref.[441],[447],[448].
Variations in alloy chemical composition can exist in different specification systems for equivalent
alloys.Careshouldbeexercisedwhencomparingalloysacrossdifferentstandardssystems,Ref.[44
6].

437

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Table44.21Magnesiumalloys:Nominalchemicalcompositions
Alloy

Composition,wt%
Al

Mn

Zn

Zr

Notes
Rare
earths

ASTM No.

UNS No.

Other

(a)

AZ63A

M11630

0.15

AZ81A

M11810

7.6

0.13

0.7

AZ91E

M11918

8.7

0.13

0.7

AZ92A

M11920

0.1

EQ21A

M12210

0.7

2.25(c)

1.5 Ag

EZ33A

M12330

2.55

0.7

3.25

...

K1A

M18010

0.7

...

...

QE22A

M18220

0.7

2.15(c)

2.5 Ag

WE43B

M18432

0.7

3.0(d)

4.0 Y

WE54A

M18410

0.7

3.5(d)

5.2 Y

ZC63A

M16331

0.25

2.7 Cu

ZE41A

M16410

4.25

0.7

1.25

ZK51A

M16510

4.55

0.7

AM20

2.0

0.40

0.20 max

AM50A

M10500

4.9

0.26

0.20 max

AM60B

M10602

0.24

0.20 max

AE42

0.50 max

0.20 max

2.5

AS21

0.4

1.0 Si

AS41B

M10412

4.25

0.35

0.12

1.0 Si

AZ91D

M11916

0.15

0.7

AZ10A

M11100

1.2

0.2

0.4

AZ31B

M11310

0.2

E
F, S, E

AZ61A

M11610

6.5

0.15

0.95

F, E

AZ80A

M11800

8.5

0.12

0.5

F, E

LA141A

M14141

1.25

0.15

14 Li

S, E

M1A

M15100

1.6

0.3 Ca

WE43B

M18432

0.7

4.0 Y

F, E

WE54A

M18410

0.7

5.2 Y

F, E

ZE10A

M16100

1.25

ZK31

0.7

0.17
-

F, E (g)

ZK60A

M16600

5.5

0.7

F, E

ZM21

1.0

2.0

S, E

Sandandpermanentmouldcastings

(b)

(e)

Diecastings

(b)
(f)

Wroughtproducts

3.0(d)
3.5(d)

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ECSSEHB3220Part4A
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Recentalloys
Sandandpermanentmouldcastings

Notes

Elektron
21
MRI-201S

M12310

0.3

0.7

4.5(h)

MRI-202S

AE44

0.50 max

0.20 max

AJ52X

4.9

0.3

1.3 Sr

AJ62

6.3

0.4

2.5 Sr

AS31

3.5

0.50 max

0.20 max

1.0 Si

MRI-153M

MRI-230D

(j)
(j)

Diecastings
(k)
(l)
(m)
(k)
(j)
(j)

Wroughtproducts
Elektron
675
Key:

(n)

(a)

Magnesiumalloyscontainingthorium(codeletterH)additionshavebeenremovedfromthis
Handbook,duetoconcernsoverresidualradioactivity,butmaystillbeavailableto
specialorderforreplacementpurposes.

(b)

Highpurity(lowFe,Ni,Cu)versionsforimprovedcorrosionresistance

(c)

Rareearthelementsareintheformofdidymium(amixtureofrareearthelementsmadechieflyof
neodymiumandpraseodymium).

(d)

Rareearthsare2.0to2.5%and1.5to2.0%NdforWE43AandWE54A,respectively,withthe
remainderbeingheavyrareearths.

(e)

ElektronRZ5

(f)

F,forging;S,sheetandplate;E,extrudedbar,shape,tube,andwire.

(g)

ElektronZW3

(h)

Proprietaryalloy,MagnesiumElektron,rareearthsare3.0%Nd,1.5%Gd

(j)

Proprietaryalloy,DeadSeaMagnesium,compositionnotpublished

(k)

Proprietaryalloy,HydroMagnesium

(l)

Proprietaryalloy,NorandaMagnesium,typicalcomposition

(m)

Proprietaryalloy,NorandaMagnesium,licensedtoMagnesiumElektron

(n)

Developmentalloy,MagnesiumElektron,compositionnotpublished

Many magnesium alloys have also been registered with SAE International for an aerospace, AMS,
standard. Like many former defence standards these apply to specific temper conditions and forms
andaretooextensivetobeincludedinthishandbook.
European standards and specifications (EN) are being developed and adopted. These are
progressivelysupersedingthevariousNationalstandardsinmemberstates,Ref.[446].
Aerospace EN specification designations are controlled by AECMA and also apply to a particular
alloy,conditionsandforms,e.g.prEN2731MagnesiumalloyMGC46001T6Sandcasting

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ECSSEHB3220Part4A
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44.2.2

Mechanical properties

44.2.2.1

Room temperature properties

Table44.2.2givestypicalroomtemperaturemechanicalpropertiesforavarietyofmagnesiumalloys.
Recentalloysareincluded,Ref.[441],[447],[448].

[Seealso:Table44.1.1foralloydesignationsystem]

Table44.22Magnesiumalloys:Typicalmechanicalproperties,atroom
temperature
Alloy

Yieldstrength

Tensile
strength

Tensile

Compressive

MPa

MPa

MPa

Bearing

Elongation
in50mm

Shearstrength

MPa

MPa

145

Sandandpermanentmouldcastings
130
130
360

AZ63A-T6

275

AZ81A-T4

275

83

83

305

15

125

AZ91E-T6
AZ92A-T6

275

145

145

360

145

275

150

150

450

150

EQ21A-T6

235

195

195

152

EZ33A-T5

160

110

110

275

145

K1A-F

180

55

125

19

55

QE22A-T6

260

195

195

WE43B-T6

250

180

187

162

WE54A-T6

280

205

172

150

ZC63A-T6

210

125

ZE41A-T5

205

140

140

350

3.5

160

ZK51A-T5

205

165

165

325

3.5

160

Elektron 21T6
MRI-201S-T6

280

170

168

172

260

170

190

MRI-202S-T6

250

150

145

AM20

206

94

16

AM50A

220

120

113

6 - 10

AM60B

220

130

130

6-8

AS21

230

120

106

12

AS41

240

130

10

AE42

237

134

103

8 - 10

AZ91D

230

150

165

140

AE44

245

142

10

AJ52X

232

145

AJ62

227

138

Diecastings
74

440

ECSSEHB3220Part4A
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Yieldstrength

Alloy

Tensile
strength

Tensile

Compressive

Bearing

Elongation
in50mm

Shearstrength

AS31

MPa
216

MPa
130

MPa
-

MPa
-

%
8

MPa
-

MRI-153M

250

170

170

MRI-230D

235

180

180

AZ31B-H24

290

220

180

325

15

160

LA141A-T7

145

125

23

ZE10A-H24

234

152

ZM21-H14

250

165

5-8

AZ10A-F

240

145

10

AZ31B-F
AZ61A-F

260

200

97

230

15

130

310

230

130

285

16

140

AZ80A-T5

380

275

240

165

LA141A-T7

139

108

23

...

M1A-F

255

180

83

195

12

125

WE43B-T6

270

190

10

WE54A-T6

275

190

10

ZK31-F

305

225

200 - 250

145

ZK60A-T5

365

305

250

405

11

180

ZM21-F

230

150

Elektron 675

400

300

130 - 165
-

6
7

Sheetandplate

Extrudedbarsandshapes
69
-

(a)

Forgings
AZ61A-F

275

160

AZ80A-T5
WE43B-T6

290
280

200
180

WE54A-T6

295

195

ZK31-F

290

205

165 - 215

ZK60A-T5

365

305

250

405

11

180

Key:

(a)Developmentalloyprovisionaldata

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44.2.2.2

Low temperature properties

Magnesiumalloysdonotundergoductilebrittletransitionandlowtemperatureductilityshowonly
smallfallscomparedwithroomtemperaturevalues.Someexamplesoftensilepropertiesat196C are
given in Table 44.2.3.

Table44.23Magnesiumalloys:Typicallowtemperaturetensilepropertiesat
196C
Alloy

Yieldstrength

Tensilestrength

Elongation

MPa

MPa

Castalloys
AZ91C-T6

180

310

1.7

AZ92A-T6

195

320

0.8

EZ33A-T5

154

QE22A-T6

233

359

2.4

ZE41A-T5

245

Elektron 21-T6

270

460

Wroughtalloys
ZK31-F

44.2.2.3

Elevated temperature properties

Typicaltensilepropertiesofanumberofmagnesiumalloysattemperaturesupto300C are given in


Table 44.2.4.

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Table44.24Magnesiumalloys:Typicaltensilepropertiesatelevated
temperatures
Testtemperature
150C

Alloy

YS
(MPa)

200C

UTS
(MPa)

YS
(MPa)

250C

UTS
(MPa)

YS
(MPa)

300C

UTS
(MPa)

YS
(MPa)

UTS
(MPa)

55 (b)

55 (b)

AZ63A-T6

AZ92A-T6

EQ21A-T6

180

SandandPermanentMouldCastings
165
110 (a)
195
115
(a)
211
191
152
169
170

EZ33A-T5

85

140

75

130

70

110

55

85

QE22A-T6

208

260

170

215

80 (b)

185

145

WE43B-T6

245

115

155

WE54A-T6

195

255

183

241

175

230

140

180

ZE41A-T5

120

170

100

135

80

110

55

85

MRI-201S

170

245

MRI-202S

145

220

Elektron 21T6

165

255

160

240

145

185

95

155

132 (b)

Diecastings
AE42
AS21

75

130

AS41

85

152

AZ91D

110

159

AJ62
MRI-153M

135

190

MRI-230D

150

205

AZ80A-T5

235

WE43B-T6

185

Extrusions
170

235

130

210

69 (b)

175

240

165

230

WE54A-T6

185

245
250

ZK31-F

100

150

50

125

15

100

ZK60A-T5

180

41 (b)

Elektron
675

290

380

95

150

60

Sheet
105

40

65

48 (b)

AZ31B-H24
Key:

(a)Testedat205C;(b)Testedat315C

Magnesium alloys generally show a rapid fall off in strength above 150C and much of the
development work has centred on improving this situation. The sand casting alloys based on rare
earthadditions,e.g.WE43andWE54,havelargelyovercometheproblemswithearlieralloysandthe
newer alloy, Elektron 21, shows good promise as a lower cost alloy with good corrosion resistance.

443

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WE54showsalossofductilityafter>5000hoursatelevatedtemperaturesandwherethismightbea
problemalloyWE43ispreferred.
ForextrudedproductstheWEalloysalsoshowthebestperformanceamongsttheestablishedalloys
but recent work by Magnesium Elektron has resulted in a new alloy, Elektron 675, with high
temperature strength exceeding that of many aluminium alloys. Preliminary data for this alloy is
provided,[See:Table44.2.4].
The WE alloys and Elektron 21 also show the best longer term creep properties, as shown in Table
44.2.5
Thenewerdiecastingalloyshavebeendevelopedforimprovedelevatedtemperaturepropertiesand
although the short term tensile properties are not much different from AZ91 they show improved
longertermcreepresistance.

Table44.25Magnesiumalloys:Typicalelevatedtemperaturecreepproperties
TestTemperature
Alloy

150C

200C

250C

Stress(MPa)toproduce0.2%strainin1000hours
SandandPermanentMouldCastings
EQ21A-T6

134

52

19

EZ33A-T5

57

20

WE43B-T6

110

37

WE54A-T6

170

35

ZE41A-T5

80

15.5

Extrusions
ZK31-F

17
Sheet

AZ31B-H24

17

Stress(MPa)toproduce0.1%strainin100hours
SandandPermanentMouldCastings
AZ92A-T6

12

WE43B-T6

150

ZE41A-T5

40

Elektron 21-T6

100

Diecastings
AE42

65

40

20

AS21

38

30

AS41

15

15

AZ91D

20

444

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44.2.2.4

Fatigue and fracture toughness properties

Fatiguedataformagnesiumalloyshas,formanyyears,beenlimited,Ref.[447].Thishasbecomea
requirement for their application in automotive and aerospace sectors. However, magnesium alloys
aresimilartootheralloysinthatfatiguestrengthdependsontensilestrength,Ref.[4411].Theratiois
not so well defined as for some other metals since whilst solidsolution strengthening increases the
fatigue strength of magnesium alloys, cold working and precipitation strengthening produce little
improvementinfatiguestrengthatlongerlives.
When compared with data for A357 aluminium alloy, SN curves for AZ91E and WE43 show that
although A357 performs well at low cycles the situation changes so that WE43 has the better
propertiesathighcycles.Thelowerstrengthalloy,AZ91E,haslowerpropertiesatlowcyclesbutat
highcyclesthedifferencecomparedwithWE43islessmarked,Ref.[4411].
RoomtemperaturefatiguestrengthsofsomemagnesiumalloysaregiveninTable44.2.6togetherwith
fracturetoughnessKIcvalues.

Table44.26Magnesiumalloys:Typicalfatigueandfracturetoughnessproperties
atroomtemperature
Alloy

Fatiguestrength(a)

Fracturetoughness,K1C

MPa

MPam

SandandPermanentMouldCastings
AZ91E-T6

70

13.2

AZ81A-T4

70

EQ21A-T6

100 - 110

16.4

EZ33A-T5

60

WE43B-T6

80

15.9

WE54A-T6

97

14.3

ZE41A-T5

100

15.1 - 16.3

Elektron 21-T6

115 - 120 (b)

15

Diecastings
AZ91D

70

AM50A

70

AM60B

70

Extrusions

ZK31A-F

122

45.6

WE54A-T5

145

15 - 17

Elektron 675 (d)

200 (b)

Sheet

AZ31B-H24
Key:

100 (c)

(a)

510 cycles,rotatingbendtest

(b)

5107cycles,pullpulltest,R=0.1(ASTME466)

(c)

5107cycles,cantileverbendtest

(d)

Developmentalloy,provisionaldata

28

445

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Inadditiontoalloymanufacturersfatiguedata,astudyconsideredthefatigueperformanceofseveral
recentalloys(AM50,AM60,AE42,WE43andRZ5),Ref.[447]:

S-N curves for round bar and flat specimens.

IST - incremental step test and hysteresis effects.

Stress-lifefunctions(stressamplitudeversusfatiguelife)forroundandflatspecimensofWE43
andRZ5alloys.

44.2.2.5

Damping capacity

Magnesiumalloysingeneralshowhigherdampingcapacitythanmostcommonstructuralmetals.
InparticularmagnesiumalloyK1AshowsaspecificdampingcapacityaroundtwicethatoftheCu
Mndampingalloysandsixtimesbetterthangreycastiron,showninTable44.2.7.
MagnesiumK1Athereforefindsaerospaceapplicationswherevibrationdampingisimportant.

Table44.27Magnesiumalloys:Dampingcapacityofselectedalloys
andothermetals
Alloy

Specificdampingcapacityat10%ofyield
stress
Castalloys

K1A

60

AZ91E

0.2

AZ80A-T4

0.02

EQ21A-T6

0.22

EZ33A-T5

4.5

WE43B-T6

0.09

WE54A-T6

0.17

ZE41A-T5

1
Othermetals

1100 aluminium

0.3

2011 aluminium alloy

0.25

Other Al alloys

<0.2

Grey cast iron

10

Cu-Mn damping alloys

20 - 40

44.3

Discontinuously reinforced magnesium composites

44.3.1

Types of discontinuous reinforcement

Discontinuousreinforcementsformagnesiumalloysaregroupedas:

Particulates, using additions silicon carbide or boron carbide particles

Short ceramic fibres, using alumina or carbon.

Whiskers, using silicon carbide.

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44.3.2

Effect of particulate additions

Theadditionofparticulatestoabasemagnesiumalloy:

Increasestheinitialtensilemodulus,

Increasesyieldandtensilestrengths,providedmodestadditionsofparticlesaremade.

Reduceselongation,fortheoptimisedcompositeswith12to15volumepercentageparticles.

Reduction of CTE, from 26 106 /C to 20 106 /C, for a 20% addition of silicon carbide
particles.

44.3.3

Processing

44.3.3.1

General

In the USA,atomised ZK60A alloy inpowder form has been consolidated with both SiC and boron
carbideparticles.
MagnesiumElektron(UK),preferthecheapermeltstirringroutetocreatethecompositeusingZC63
andAZ91castingalloysorvariantsonZC71wroughtalloy,Ref.[4417].
Shortfibreandwhiskerreinforcedcompositesareusuallypreparedbymeltinfiltrationofpreformsby
squeezecastingorpressurediecastingtechniques,Ref.[4414].

44.3.3.2

Occupational health and safety

ManytypesofceramicwhiskersandpolycrystallinefibreshavebeenevaluatedbytheWorldHealth
Organisations International Agency for Research on Cancer (Monograph 43, 1988) as possibly
carcinogenic to humans, and are subject to occupational health and safety risk control measures in
somejurisdictions.
Exposuretorespirabledustscontainingthesematerialsshouldbeavoided.Suchdustsarenotlikelyto
bereleasedfromMMCsintheirnormalhandlinganduse,butcontrolmeasuresneedtobetakenifthe
materialsaremachined,cutorsubjecttoabrasion.
RefertomanufacturersandsuppliersSafetyDataSheetsforfurtherhealthandsafetyinformation.

44.3.4

Properties

RepresentativepropertiesoftheSiCreinforcedAZ61alloycompositearegiveninTable44.3.1.

Table44.31SiCparticulatereinforcedAZ61magnesiumalloy:Typical
mechanicalproperties
Material

AZ61
AZ61 + 2%SiC
AZ61 + 5%SiC

Modulus

0.2%PS

UTS

Elongation

(GPa)

(MPa)

(MPa)

(%)

44
60
66

190
242
261

290
310
321

18
2.0
1.2

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ECSSEHB3220Part4A
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For highstrength, highrigidity applications, Magnesium Elektron MELRAM 072 contains 12%SiC
(10mmeanparticlesize)usingamatrixbasedontheZC71alloy.
Toimprovetheextrudabilityandroomtempertatureductility,thematrixcompositionwasmodified
to Mg4.5%Zn0.5%Mn, and the extruded product given a cold drawing operation, which also
improveddimensionalaccuracy.ThismaterialwasrenamedMELRAM072TS.
TypicalmechanicalpropertiesforbothvariantsareshowninTable44.3.2,Ref.[446].

Table44.32SiCparticulatereinforcedmagnesiumalloy:Typicalmechanical
properties
Material(1)

MELRAM 072
ZC71 + 12%SiC
MELRAM 072TS
Mg-4.5%Zn-0.5%Mn +
12%SiC
Key(1):

Modulus

YS

UTS

Elongation

(GPa)

(MPa)

(MPa)

(%)

63

370

398

1.5

63

311

344

MELRAMMagnesiumElektron,developmentMMC(1998).

44.4

Continuously reinforced magnesium composites

44.4.1

Types of composite

Thetypesofcontinuousreinforcementconsideredformagnesiumalloysare:

carbonfibre,

siliconcarbidefibre.

Workhascentredoncontinuouscarbonfibrereinforcedmagnesiumalloys.
Table44.4.1showsexamplesofMMCs,Ref.[442],[443],[444],[445],[4416],[4418].

Table44.41ContinuousfibrereinforcedmagnesiumMMCmaterials:Examples
Fibre

Matrix

Comments
Carbonfibre

T300

Mg-1Al

M40
K63B12

Mg 99.85
AZ31

P55

AZ91C

P100

AZ31B
AZ61A

Squeeze cast.
Susceptible to galvanic corrosion.
Gas pressure infiltration
Gas pressure infiltration
Design for near zero CTE.
Laser absorptivity tests.
Siliconcarbide

SCS-2

ZE41

Cast rod.

448

ECSSEHB3220Part4A
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44.4.2

Features

CarbonfibrereinforcedmagnesiumMMCsoffer:

high specific properties, and

possibility of near-zero thermal expansion characteristics.

Consequentlytheyhavebeenconsideredashavingpotentialusesinaerospaceapplications,Ref.[44
2],[4416],[4418].

44.4.3

Processing

The starting point for all continuous fibrereinforced magnesium composites is a fibre preform. The
mostpopularproductionmethodisfilamentwindingalthoughweaving,knittingandvariantsthereof
arealsoemployed.Tosomeextentthechosenmethoddependsonthetypeofcarbonfibreused.
The magnesium matrix is incorporated by molten metal techniques which depend upon the chosen
typeofpreform.Thus,topreventdamagetofilamentwoundpreformstheseareusuallygaspressure
infiltratedwhilstwovenorknittedpreformsareusuallymorerobustandsqueezecastingorpressure
diecastingtechniquesmayalsobeemployed.
In carbonMg MMCs the properties are dictated primarily by the reinforcement, the matrix serving
mainly to hold the fibres together. The important factors are therefore the nature of the bonding
betweenfibreandmatrixandtheavoidanceofanydegradationoffibrepropertiestointeractionwith
the matrix. These are therefore prime factors in the selection of the matrix alloy although prior
treatmentsmayalsobeappliedtothefibresurfaces.

44.4.4

Properties

Table44.4.2givesgeneralmechanicalpropertydataonmagnesiumMMCmaterials,Ref.[441],[443],
[444],[4418].
Themaininterestincarbonfibrereinforcedmagnesiumcompositesforspaceapplicationsappearsto
be in materials with low CTE coefficient of thermal expansion, together with high thermal
conductivity.
Published information is sparse, but data from USbased work indicates CTE of 1.67ppm/K with
conductivityof180W/mKcomparedwith0.5ppm/Kand1.5W/mkforfusedsilicaand26ppm/Kand
122W/mKforpuremagnesium,Ref.[4416].

449

ECSSEHB3220Part4A
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Table44.42MagnesiumcontinuousreinforcedMMCs:Typicalmechanical
properties
Composite

Fibre
vol.
(%)

P55/AZ91C+AZ31B faces
P55/AZ91C+AZ31B faces
P100/AZ91C+AZ31B faces

12.7
23.3
28.4

P100/AZ91C+AZ61A faces

37.0

T300/MgAl1

45

M40/Mg

65

SCS-2/ZE41

34
46
50
37

Typicalproperties
UTS
(MPa)

E
(GPa)

Carbonfibre
367
85.5
543
135
574
237
489
290
284
258

Failure
strain(%)

Comments

0.29
0.48
0.42
-

Single ply
Three ply
Single ply
RT/Tensile
RT/Compressive
149C/Compressi
ve
260C/Compressi
ve
Longitudinal
Transverse
-

294

247

214

263

440
150
1500

105
30
235

Siliconcarbide
1000
169.6
1524
209.6
1331
230.3
1379
180.6

0.83
0.88
0.78
0.95

675C/5 mins
675C/10 mins

44.4.5

Environmental resistance

44.4.5.1

Galvanic corrosion

Magnesium MMCs suffer from one severe problem in that they are highly susceptible to galvanic
corrosion;thisisduetothepotentialdifferencebetweenfibreandmatrix.
A study on the corrosion of T300 carbon fibres in Mg1Al alloy showed corrosion occurred in a
laboratoryenvironmentandcorrosivepenetrationwasintheorderof100mperyear,Ref.[442].
Further studies have shown, however, that both the selection of matrix alloy and fibre coating
techniquescanreducedetrimentalcorrosioneffects.
Galvanic corrosion can be controlled by proper and adequate protection methods, such as painting.
Such protection methods rely on being intact and not disrupted during the entire manufacturing,
assembly,storageandservicelifeofthefinisheditem,Ref.[4419].
Whilstthemechanicalandthermalexpansionofthesematerialsshowspromiseforspaceapplications,
considerableeffortisneededtoreducethecorrosionaspectsandproductioncosts.

[Seealso:ECSSQ7071]

450

ECSSEHB3220Part4A
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44.5

Potential applications

44.5.1

Alloys

Theverylowdensityofmagnesiumisanobviousattraction,andalthoughthestiffnessandstrengths
ofthealloysaremodest,thesearegoodwhenconsideredonaspecificbasisi.e.strengthtoweight
ratio.SatelliteapplicationshaveusedAZ31,AZ61(AZM),AZ80andZK60alloys.
A MgLi development alloy, Ref. [4412], has a very low specific gravity of 1.35, although it never
reachedcommercialstatusandisnowobsolete.However,workcontinuesonotherMgLialloysand
compositesbaseduponthem,Ref.[4413],[4414].
[Seealso:ECSSQ7071]
Conventional alloy developments have increased properties at elevated temperatures, e.g. RZ5
(ZE41A)to130C;WE43andWE54to300C(shortterm)and250C(longterm)andtheneweralloy
Elektron 21 shows excellent promise. These alloys are finding uses in applications such as
transmissioncasingsformilitary,civilaircraftandhelicopters,Ref.[448].
Magnesium Elektron have recently announced the development of a new extruded alloy, Elektron
675,whichisclaimedtohavegreaterstrengthattemperaturesabove100Cthanwrought2000series
and 7000series aluminium alloys. At 200C, yield strength is 290MPa, and the ultimate tensile
strengthis380MPa.Thisisover100%strongerthan2024aluminium,andmorethan200%stronger
than7075.

44.5.2

Composites

Improvementsinstiffnesscanbeachievedbytheadditionoffibresandparticlestogivecomposites.
Specialised components can be made in continuous fibre composites, mostly with carbon fibre for
dimensionalstability.However,forlonglifestructures,thecorrosioncharacteristicsofmagnesium
based composites causes concern and the economics of production of these materials has mitigated
againsttheirdevelopmentandwideravailability.
The field of metalmatrix composites is still relatively new and rapidly developing. To assist the
engineerinupdatinginformationontechnologyandpotentialsuppliersaThematicNetworkentitled
MMCAssesshasbeenestablishedwithE.C.fundingandisadministeredbytheUniversityofVienna.
Itprovidesengineerswiththestatusofthesematerials.

44.5.3

Space

44.5.3.1

General

Magnesiumalloysaremostlikelytobeusedintheformofmachinedcastings,forgingsorextruded
rod or bar. However, as in the case of aluminium alloy aerospace components, there is a growing
trendtouseextrudedbilletforforgingstockorforprecisionmachiningforlongercomponents.
Given the mandatory limitations imposed on the use of magnesium materials in space, possible
applicationsremain:

Dimensionallystabletubesandstruts.

Endfittingsandconnectionsforlatticestructures.

Mirrorsubstrates.

451

ECSSEHB3220Part4A
20March2011

44.5.3.2

Satellite

Figure44.5.1showsamagnesiumalloymomentumwheelbracketforasatellite.Thisitemis250mm
150 mm 80 mm and was machined from ZK60A-T5 extruded bar and treated with ALGAN 2 plus
OXSILANMG0611,Ref.[4422].

Thisitemis250mm 150 mm 80 mm and was machined from ZK60A-T5 extruded bar and treated with
ALGAN2plusOXSILANMG0611,Ref.[4422].

Figure44.51Magnesiumalloys:Momentumwheelbracketforsatellite
Example

44.5.3.3

Mirrors

Magnesiumbased composites are under consideration for light weight mirrors. MetGraf Mg is a
tradenameofMMCC(USA)
Figure 44.5.2 shows an example of a carbonreinforced magnesium alloy lattice structure used to
supportsiliconbasedreflectors,Ref.[4416].

452

ECSSEHB3220Part4A
20March2011
Attachment of Si and SiC membranes to
Lightweighted MetGraf Mg substrates with pre and post polishing options

Pre-polished Si membrane bonded to lightweighted


substrate.

SiC membrane bonded to Mg/Carbon lightweighted


substrate.

Areal density = 9.7 kg/m 2

Part to be Si coated and polished

Figure44.52Carbonfibrereinforcedmagnesiumalloy:Spacemirrors
(experimental)Example

44.6

References

44.6.1

General
[441]

PropertiesandSelection:NonferrousAlloysandSpecialPurpose
Materials
ASMHandbook,10thEdition,Volume2
ASMInternational.ISBN0871703785(V.2)

[442]

B.J.Macleanetal
ThermalMechanicalBehaviourofGraphite/MagnesiumComposite
MartinMariettaAerospaceProceedingsofSymposiumonMechanical
BehaviourofMetalMatrixComposites
Dallas,Texas.February16thto18th,1982

[443]

I.W.Hall
CorrosionofCarbon/MagnesiumMetalMatrixComposites
UniversityofDelawareScriptaMetallurgica.Vol.21,1987

[444]

D.J.Changetal
CompressivePropertiesandLaserAbsorptivityofUnidirectionalMetal
MatrixComposites
TheAerospaceCorporationReportNo.SDTR8681
30thSeptember1986

[445]

EngineeredMaterialsHandbook.Volume1.COMPOSITES
ASMInternational,MetalsPark,Ohio

453

ECSSEHB3220Part4A
20March2011
ISBN0871702797(v.1)
[446]

B.Hussey&J.Wilson:RJTechnicalConsultants,UK
LightAlloysDirectory&Databook
Chapman&Hall(1998).ISBN0412804107

[447]

HJ.Ertelt:ISDInstituteforStatics&Dynamics,D
SomeFatiguePropertiesofMagnesiumAlloys
ProceedingsofESAEuropeanConferenceonSpacecraftStructures,
Materials&MechanicalTesting,Braunschweig,D.46November,1998.
ESASP428,p263268

[448]

ExtractfromMagnesiumElektronwebsite:www.magnesium
elektron.com(April2003).

[449]

DataSheet256,SurfaceTreatmentsforMagnesiumAlloysinAerospace
&Defence
MagnesiumElektron,1997:www.magnesiumelektron.com

[4410]

DataSheet254,MachiningMagnesiumAlloys
MagnesiumElektron,2000:www.magnesiumelektron.com

[4411]

FatigueandFracture
ASMHandbook,volume19
ASMInternational.ISBN0871703858

[4412]

NASASP5028,
TechnicalandEconomicStatusofMagnesiumLithiumAlloys,PaulD.
Frost,August1965
http://ntrs.nasa.gov/archive/nasa/casi.ntrs.nasa.gov/19650020351_1965020
351.pdf

[4413]

F.W.Bachet.al.
SFB390PrjectA4:DensityReducedMagnesiumAlloyswithIncreased
Ductility
UniversityofHanover,Germany
http://www.iw.unihannover.de/sfb/sfb390/englisch/index_e.html

[4414]

S.Kudela
Magnesiumlithiummatrixcompositesanoverview
Int.J.ofMaterials&ProductTechnology,Vol.18,Nos1/2/3,2003,p91
115

[4415]

A.A.Luo
Recentmagnesiumalloydevelopmentsforelevatedtemperature
applications
InternationalMaterialsReviews,2004,Vol.49,No1,p1330

[4416]

J.A.Cornie,L.Ballard,E.Chen&S.Zhang
Developmentofgraphitefiberreinforcedmagnesiumalloysfor
lightweightmirrorsubstratesandzeroCTEmeteringstructures

454

ECSSEHB3220Part4A
20March2011
NationalSpace&MissileMaterialsSymposium:Seattle,2125June2004
LINK

44.6.2

[4417]

J.F.King,T.E.Wilks&G.D.Wardlow
PropertiesandapplicationsofmagnesiumMMCmaterials
IMA53,conf.Proc.,Ube,Japan,1996,p7782

[4418]

A.Schoberth
Overviewoncontinuousfibrereinforcedlightmetals
MMCVIII,MetallicComposites&Foams,26/27.11.2001,TheInstituteof
Materials,London
http://mmcassess.tuwien.ac.at/public/cont_fibers.pdf

[4419]

A.Schoberth
ContinuouscarbonfiberreinforcedMgalloys
paperinmmcdatasectionofMMCAssesswebsite
http://mmcassess.tuwien.ac.at/index1.htm

[4420]

ASTMB27504:StandardPracticeforCodificationofCertainNonferrous
MetalsandAlloys,CastandWrought
ASTMInternational,100BarrHarborDrive,POBoxC700,West
Conshohocken,PA194282959,USA

[4421]

ASTME52783(Reapproved2003):StandardPracticeforNumbering
MetalsandAlloys(UNS)
ASTMInternational,100BarrHarborDrive,POBoxC700,West
Conshohocken,PA194282959,USA

[4422]

AMTS(Israel)privatecommunication(2005)

Sources
Alubin:www.alubin.com
AMTS,WroughtProductDivision:www.magnesiumtechnologies.com
DeadSeaMagnesium:www.dsmag.co.il
HydroMagnesium:www.hydromagnesium.com
MagnesiumElektron:www.magnesiumelektron.com
OttoFuchs:www.ottofuchs.com
Timminco:www.timminco.com

44.6.3

Organisations
InternationalMagnesiumAssociation:www.intlmag.org
IsraeliConsortiumfortheDevelopmentofMagnesium:www.dmtc.org.il
MMCAssess:mmcassess.tuwien.ac.at

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44.6.4

ECSS standards
[See:ECSSwebsite]

ECSSQ7071
ECSSQST7036

ECSSQST7037

44.6.5

Datafortheselectionofspacematerialsand
processes;previouslyESAPSS01701
Materialselectionforcontrollingstress
corrosioncracking;previouslyESAPSS01
736
Determinationofthesusceptibilityofmetals
tostresscorrosioncracking;previouslyESA
PSS01737

ASTM standards
[See:ASTMwebsite]

ASTMB27504
ASTME52783

StandardPracticeforCodificationofCertain
NonferrousMetalsandAlloys,CastandWrought
StandardPracticeforNumberingMetalsand
Alloys(UNS).Reapproved2003

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45
Copper alloys and their composites
45.1

Introduction

Copper alloys are not considered for structural applications, unless the application has exacting
electricalorthermalconductivityrequirements.
Themechanicalpropertiesofthealloyscanbeimprovedbyusingreinforcement,buttheconductivity
oftensuffersasaresult.
Some copper alloys exhibit a shape memory effect. These alloys, sometimes known as smart
materials,canbeusedasactuators,[See:91.5].

45.2

Copper alloys

45.2.1

Precipitation hardening

Therangeofcopperalloysislarge,Ref.[451].Thosealloyswhichareofpreliminaryinterestinclude
the precipitationhardened systems which have enhanced strengths without loss of conductivity.
Thesealloysinclude:

CuBe,

CuAg,

CuZr,

CuCr.

AnexampleisNarloyZ.
These alloys form the baseline for many industrial applications, but can be considered as lacking in
certainareasofpropertyoptimisation;mostnotablyhightemperaturecreepresistance(~500C)and
dimensional stability. This has initiated some reinforced copper and composite developments
appropriatetospaceapplications.

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45.3

Copper ODS alloys

45.3.1

Types and effects of dispersions

Addingveryfinedispersionsofalumina(Al2O3)andtitaniumdiboride(TiB2),inlowconcentrations,
hasachievedsignificantimprovementsinselectedpropertiesoverprecipitationhardenedsystems.
CopperODSalloysarepreparedbyapowderroute.

45.3.2

Properties

Whilstmaintaininggoodconductivity,thehardness,wearresistanceandcreepresistancehavebeen
improved. This is most noticeable in the retention of strength to higher temperatures than the
conventionalalloys,asshowninFigure45.3.1.

Figure45.31CopperODSalloys:Elevatedtemperaturestressruptureproperties
ofGlidcopODSalloyscomparedwithsomehighconductivitycopperalloys

Table 45.3.1 gives the ambient temperature properties attainable by ODS alloys, whilst Table 45.3.2
andTable45.3.3providedataat538C.

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Table45.31CopperODSalloys:Ambienttemperaturetensileproperties
Material/Temper

Modulus
(GPa)

[See:Key]

Proofstress

UTS(MPa)

0.2(MPa)

Straintofailure
(%)

Cl5710:Cu+0.2wt.%.Al203,

As fabricated
Cold worked 98.5% RA

105
106

270
540

325
565

20
-

470
615

19
3.5

485
585

16
10

15720:Cu+0.4wt.%.Al203,

As fabricated
Cold worked 98% RA

113
113

365
585

Cl5735:Cu+0.7wt.%.Al203,

As fabricated
Cold worked 56% RA

123
123

420
565

Cl5715,GlidcopAl15:Cu+0.3wt.%.Al203

As hipped
As extruded
Extruded + 98% cold
work

130
130

255
331

360
413

26
20

130

613

661

Cl5725,GlidcopAl25:Cu+0.5wt.%.Al203,

As hipped
As extruded
Extruded + 98% cold
work

130
130

295
345

410
4,34

18
21

130

613

675

GlidcopAl25:Cu+0.5wt.%.Al203,

As hipped
As extruded

130
130

413
655

517
737

13
6

SutekMXT5Cu+5vol.%TiB2

Extruded and cold


rolled
8% reduction in
thickness

620

Key:

ASMMetalsHandbook,10thEdition,1990.

Manufacturersdata,SCMMetalProductsInc,USA.

Manufacturersdata,SutekCorp,USA.

675

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Table45.32CopperODSalloys:Shorttermpropertiesat538C
Material

C15715,GlidCop Al-15:
Cu-0.3 wt.%Al2O3
C15725,GlidCop Al-25:
Cu-0.5 wt.%Al2O3
Sutek MXT-5A:
Cu-5 vol.% TiB2
Key:

Temper

YS0.2

UTS

(MPa)

(MPa)

(%)

As HIP

85

85

As HIP

105

120

Unknow
n

145

145

Manufacturersdata:SCMMetalProductsInc.,USA.
Manufacturersdata:SutekCorporation,USA.

HIP:Hotisostaticpressing

Table45.33CopperODSalloys:Creepstrengthat538C
Material(Tempernotstated)

C15715, GlidCop Al-15:


Cu-0.3 wt.%Al2O3
C15760, GlidCop Al-60:
Cu-1.1 wt.%Al2O3

100hrCreeprupturestrength(MPa)

190
260

45.4

Discontinuously reinforced copper composites

45.4.1

General

Thereisvirtuallynopublishedinformationontheuseofparticleordiscontinuousfibrestoreinforce
copper.

45.4.2

Problems

Indicationsarethat:

Additions of inorganic, insulative phases such as SiC, Al2O3 and B4C noticeably reduce
conductivitycharacteristics.

Additionofparticlestoprecipitationhardenedsystemsislikelytoaffectthemicrostructureof
thematrixalloy.

Theadditionofparticlestopurecopperdoesnotgivesubstantialimprovementsinstrengthto
matchprecipitationhardenedorODSalloys.

Problemsariseinobtainingsatisfactorybondingbetweenparticleandmatrix,Ref.[452].

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45.5

Continuously reinforced copper composites

45.5.1

General

ThesematerialshavebeenstudiedintheUSAtoprovidesupportforthespaceprogrammes.

45.5.2

Types and effects of reinforcements

45.5.2.1

Carbon fibre

Interesthascentredoncarbonfibre(graphite)reinforcedmaterialsusingpitchfibres(AmocoP100).
Thepitchfibrescontributeto:

Thermal conductivity: The pitch fibres increase the conductivity beyond that possible with
copperalone.

Verylowcoefficientofthermalexpansion,albeitanisotropic.

45.5.2.2

Tungsten filaments

Compositeswith10%tungstenfilamentshavebeenproposedforcombustionlinerswhere:

hoop strength can be increased by 90%withonlya4%lossinconductivity.

This suggests opportunities for the copper wall thickness to be reduced to increase its heat transfer
coefficientwithoutsacrificingstrength.

45.5.3

Properties

45.5.3.1

General

Detailedinformationonmaterialsisawaited.

45.5.3.2

Thermal characteristics

Table 45.5.1 presents the thermal characteristics of fibrereinforced copper compared with carbon
fibre/aluminiumcomposites.

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Table45.51Continuousfibrereinforcedcopper:Thermalconductivityof
carbon/Cuandcarbon/Alcomposites
Thermalconductivity

CTE

(W/mK)

(ppm/C)

Material

Pure Copper
P100/Copper (UD)
P100/Copper
(0/90)s
P100/6063 Al (UD)
P100/6063 Al
(0/90)s
Key:

Long.
398
454
305

Trans.
398
140
305

Long.
16.5
2.0
5.76

Trans.
16.5
11.7
5.76

339
216

94
216

1.62
5.04

26.6
5.04

Propertiesgivenforcomparativepurposes.

Nominally40%carbonfibre.

Density
(kg/m3)

8960
5600
5700
2450
2470

45.6

Potential applications

Copper is not considered a structural material because its density is too high with respect to its
strengthandstiffness.Itsattributesmainlyrelatetoitsexcellentelectricalandthermalconductivity.
For practical systems using these conductivity characteristics there is a need to improve the
mechanical properties, notably wear resistance and hightemperature stability. Unfortunately most
methodsofachievingthistendtoimpairtheconductivity.
Twomaterialswithpossibleusesinspaceareoxidedispersionstrengthened(ODS)alloysandcarbon
(pitch)fibrereinforcedcopper.
Potentialapplicationsinclude:

Rocketenginecombustionliners.

Heatexchangersandradiators.

Spacepowersystems.

45.7

References

45.7.1

General
[451]

MetalsHandbook,Volume2,TenthEdition
PropertiesandSelection:NonferrousAlloysandSpecialPurpose
Materials
ASMInternational,ISBN0871703785(v.2),1990

[452]

J.F.Mason
ThedevelopmentofHighConductivity/ThermallyStableCopperbased
Composites
WorkOrderNo.17.BNFFulmerReportR1176/10/1
November1990forESTECContract7090/87/NL/PP

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