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ThermalAblativeExperimentation

Introduction
AblativeMaterials
PreparationofSpecimens
TestSetupandProcedure
Results
Discussion
Analysis
Conclusion
AppendixA
AppendixB

Introduction

Thisreportdescribesexperimentationthatwasperformedonvariousablativematerialstoascertaintheir
effectivenessinprovidingthermalprotectionofrocketmotorcomponents.An"ablativematerial"isa
polymerwithinherentlylowthermalconductivitywhichslowlypyrolyzeslayerbylayerwhenitssurfaceis
intenselyheated,leavingaheatresistinglayerofcharredmaterial.
Theintentofstudyingvariousmaterialswastocomeupwithasimple,readilyavailableandinexpensive
ablativeforuseinamateurrocketmotors.Theimmediateneedisforanablativethatwillservetoinsulatea
newlydesignednozzleandbulkhead,suchthatthetemperatureiskeepsufficientlylowtominimizeheating
ofacompositemotorcasingunderdevelopment.Moresothanmetalcasings,compositesaresusceptibleto
lossofstrengthandstiffnessatelevatedtemperature.
Besidestheaforementionedbasicrequirements,threespecificrequirementsofapracticalablativearebeing
sought:
1. Provideeffectiveprotectionagainstseverethermalloading.Inotherwords,thepartbeingprotected
mustbekeptbelowacertainmaximumtemperature.
2. Bereadilymoldable,machineableandpossessinggoodbondingcharacteristics.Itisenvisionedthatan
ablativematerialwouldbeappliedtothepartrequiringprotection,perhapswiththeaidofamould,
thenmachinedtoafinalthicknessordesiredprofile.
3. Resistanceto"flowdeformation"underacombinationofexposuretoheatingandhighvelocitygas.
Tothisend,itwasfeltthatafillermaterialmaybebeneficial,integratedintoaresinmatrix.
ThisstudyissimilartooneconductedinJanuary,2000andisdocumentedintheThermalProtectionfor
RocketMotorCasingswebpage.Thatsetofexperimentswasaimedatdevelopmentofaneffectivethermal
barrierforaluminummotorcasings.

Ablativematerials
Inanattempttomeetthesesoughtafterrequirements,eightresinbasedmaterialswerechosenforthisseries
oftests:
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1. Epoxy
2. Bondobodyfiller
3. Epoxy/GlassMicrospheres
4. Epoxy/HydratedMagnesiumSulfate
5. Epoxy/Milledglass,50/50
6. Epoxy/Milledglass,30/70
7. JBKwikWeld
8. BondoGlass
Adetailedexplanationofeachfollows.
1.WestSystemmarineepoxy,standard5:1resin/hardenerratio.Thismaterialwaschosentodeterminethe
effectivenessandperformanceofahighgrade,unfilledepoxy.
2.Bondobodyfillerisatwopartputtylikematerialusedforautomotivebodyrepair,itconsistsofa
polyester/styreneresinwithinertfiller.AccordingtotheMSDS,theproducthasthefollowingconstituents:
ProprietaryResin3040%
Talc2030%
Styrene1020%
Magnesiumcarbonate1020%
Sodiummetaborate510%
Acatalystpasteisaddedtocurethematerial.
3.AmixtureofWestSystemepoxycontaining15%microspheres(bymass).Microspheres,alsoknownas
microballoons,arehollowspheresofglassusedasalightweightfillerincompositematerialssuchas
syntacticfoam.Microsphereshaveaverylowbulkdensity.Individualmicrospherestypicallyhavediameters
rangingfrom10to300microns.
4.AmixtureofWestSystemepoxycontaining78%hydratedmagnesiumsulfate(bymass).Morecommonly
knownasEpsomSalts,hydratedmagnesiumsulfatehasthechemicalformulaMgSO4.7H2O,ofwhich51%
ofitsmassischemicallyboundwater.Thewaterisreleaseduponheating.Sincethermalenergyisrequired
toliberateandboilawaythewater,itwasfeltthatthismaterialcouldbeaneffectivecomponentofan
ablativeinsulator.Additionally,thesteamproducedcouldformaninsulatingfilmovertheheatedsurface.
Certainfirebarriersealants,suchas3MCP25WB+takeadvantageofthisprincipleforfireprotection.
5.AmixtureofWestSystemepoxycontaining50%milledglass(bymass).Milledglassisafinepowdered
formofglassthatisusedasafillerforcomposites.Theintendedroleofusingmilledglassistoincreasethe
ablative'sresistancetoflowdeformationandheatdegradation.
6.AmixtureofWestSystemepoxycontaining70%milledglass(bymass).Similarto(5),theintentof
tryingthisparticularformulationwastodeterminetheinfluenceofglasscontentontheablative'sresistance
toflowdeformationandheatdegradation.
7.JBWeldisapopularandversatileadhesivewithgoodstrengthandthermalresistance.JBWeldKwikis
afastcuringvariant.Itisanepoxybasedtwopartadhesive,consistingofequalpartsresinandhardener.
AccordingtotheMSDS,theresinhasthefollowingconstituents:
CalciumCarbonate4050%
IronPowder1020%
EpoxyResin3040%
AromaticHydrocarbons15%
Andthehardenerhasthefollowingconstituents:
CalciumCarbonate510%
NonfibrousTalc1525%
BariumSulfate3545%
AlkylPhenol15%
Mercaptanterminatedpolymer2030%
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AmorphousSilica15%
8.BondoGlassisafillermaterialusedforautomotivebodyrepairs.Thisproductconsistsofa
polyester/styreneresinbasedmixturecontaining10%choppedglassfibres(accordingtoMSDS).Acatalyst
pasteisaddedtocurethematerial.

PreparationofSpecimens
Alleightspecimenswerepreparedinanidenticalmanner.Theablativewasbondedtoanaluminumsheet
substrateofdimensions2"x2"(50mmx50mm).Toaidadhesion,thesurfacewasroughenedwith400grit
sandpaper,thencleanedwithlacquerthinner.Tohelpensureuniformthicknessoftheablativelayer,the
substratewasboundedbyaframemadefromwoodencraftsticks.Theresultingsizeoftheablativepatch
was1.6"x1.6"(40mmx40mm).
Theablativematerialswerepreparedbycarefullyweighingouttheconstituents,blendingthoroughly,then
applyingtothesubstrateusingaspatula.Toaidbondingofthethickerepoxybasedmaterials(specimens3
6),thesubstratewasfirstgivenalightcoatingofepoxy.Aftercuringfor24hoursatroomtemperature,the
sampleswerepostcuredinanovensetat150oF(65oC.)foronehour.Thesurfacewasthensandedsmooth
andtoaconsistentthicknessofapproximately0.050in.(1.3mm).Thethicknessofeachspecimenwasthen
carefullymeasuredwithamicrometerandrecorded.TheeightspecimensareillustratedinFigure1.
Itwasfoundthatsomeofthesampleshadasmallamountofinfusedair,whichresultedintinyairbubblesin
thefinishedspecimen.Ideally,thesamplesshouldhavebeendegassedusingavacuumchamberafter
mixing.
Alloftheablativesamplessuccessfullycuredtoafullyhardenedstatewiththeexceptionofthe
Epoxy/HydratedMagnesiumSulfate.Thisparticularmaterialhadaslightgumminesstoit.Thiswaslikely
duetotheabsorbedmoisturecontentoftheHydratedMagnesiumSulfate.Moistureisknowntoinhibitfull
curingofepoxyresin.Forfuturetesting,itmaybeadvisabletoattempttodrythematerialfirstwithaidofa
desiccant.
Priortoconductingtheheatingtestonagivenspecimen,athermocouplesensorwasattachedtothebackside
ofthesubstrateplateusingaluminumfoiltape.ThethermocouplewasatypeKChromel/alumelinterfaced
toaDVMwithtemperaturemeasurementcapability.Sampleratewasapproximately3hertz.

Figure1Ablativespecimens
Clickforlargerimage

TestSetupandProcedure
Aconventionalpropanetorchwasusedforheatingthespecimens.Thespecimenwasclampedverticallytoa
supportbasewhichalsohadasupportforthetorchnozzle,arrangedsuchthatthedistancebetweennozzle
tipandspecimenwasconsistently3.7in.(93mm).Heatingtimeforeachspecimenwas10seconds,which
wascontrolledbymeansofacountdowntimer.Ametalshieldwasplacedinfrontofthespecimenpriorto
performingeachtesttoserveasaheatshield,whichwasremovedatcommencementofheating.A
camcorderwasusedtovideotapethetemperaturereadingdisplayedbytheDVM.
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ThetestsetupisshowninFigure2.

Figure2Setupforheatingtest
Thetestprocedurewasasfollows:
Startvideocamrecording,thenfireuptorch.
Placetorchinpositionwithflamedirectedatspecimencentre
Initiatecountdowntimerandsimulteouslyremoveheatshield
Atendof10secondduration(signaledbyabeepfromtimer),quicklyremovetorch
Unclampspecimenfromsupportandplungebrieflyintobucketofwater
Afterthespecimenshadcooled,theywerephotographed,theappearanceoftheburntsurfacerecorded.The
charwasthencarefullyscrapedawayandthethicknessoftheremainingablativemeasuredandrecorded.
Inadditiontotheeightablativespecimens,thesameprocedurewasrepeatedwithanbarealuminum
specimeninordertoprovidedataforestimatingtheheatingrate.

Figure3Ablativespecimenundergoingheatingtest

Results
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Theprocedureworkedwellforalleightspecimensandgooddatawascollected.Allablativesampleshad
similarcharringwhichvariedtosomeextentincolour,textureandextent.OnlytheappearanceofSpecimen
3(epoxy/Hyd.Mg.Sulfate)wasnoticeablydifferent.Itexperiencedonlylightcharringandtheouterportion
oftheablativesurfacewasnotcharredatall.Theheataffectedsurface,inthecentre,hadabubbled
appearance.
ThemeasuredtemperatureprofileswereplottedandareshowninFigure4.Themeasuredthicknessofthe
ablativecoating,beforeandafterheating,aswellasthemeasuredablationparametersareshowninTable1.
PostheatingthicknessmeasurementsofSpecimen2and3werenotpossible,astheablativematerialof
Specimen2wascrackedandslightlydeformedinthemiddle,andbecauseoftheunevenbubbledsurfaceof
Specimen3.

Figure4Resultsoftemperaturemeasurementsrecordedduringablativeheatingtests
Photographsofthespecimenstakenimmediatelyaftertheheatingtest:
Specimens1&2(EpoxyBondobodyfiller)
Specimens3&4(Epoxy/GlassMicrospheresEpoxy/HydratedMagnesiumSulfate)
Specimens5&6(Epoxy/Milledglass,50/50Epoxy/Milledglass,30/70)
Specimens7&8(JBKwikWeldBondoGlass)

Table1Thicknessmeasurementsbeforeandafterheatingtest
Clickfortableinmetricunits

Discussion
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Fromanoverallperspective,themosteffectiveablativematerialwastheEpoxy/HydratedMagnesium
Sulfatecomposition,whichperformedappreciablybetterthanalltheothers.Thepotentialdrawbacksofthis
ablativearethe"slightlygummy"physicalproperty(whichcouldhindermachinability)andtheuneven,
bubbledsurfacethatisaconsequenceofheating.Thismaybeafactorforflowsurfaces,whichshouldbe
smooth.Asmentionedearlier,dryingoftheHydratedMagnesiumSulfatemayeliminatethegumminess.
TheEpoxy/GlassMicrospherescompositionwassecondbestwithregardtothermalprotecionand
significantlybetterthantheremainingablativematerials.Thiscompositionhasacoupleofappealing
characteristics.Ithasbeenfoundtomachineverywell,andhasaparticularlylowmassdensity.
TheunfilledEpoxyablativeperformedquitewell,asdidtheBondoglass.TheBondoglasshadan
exceptionallylowablationrate.Theremainingablatives,whicheachhadahighcontentofinertfiller,were
equallyeffectiveagainstablation,butsufferedinregardtobeinglesseffectiveinsulators.JBKwikWeld
wasleasteffectiveinthisregard,likelyduetotheironcontent,whichisagoodconductorofheat.
TheBondobodyfillerexhibitedanotableshortcomingbycrackingandpartiallyseparatingawayfromthe
substrate.

Analysis
Thetimetemperaturedataobtainedfromthebarealuminumspecimenwasusedinconjunctionwith
THERMCASsoftwaretoestimatetheconvectiveheattransfercoefficient,denotedh.Avalueofh=260
W/mKwasfoundtofitthedataquitewell.Theassumedflametemperaturewas1900oC.(3450oF.).This
valueofh=260W/mKwasthenusedasinputtoTHERMCAStoproduceatimetemperaturehistoryfor
fiveoftheablativematerialstested,basedonassumedthermalproperties.Thethreeotherablativematerials
werenotconsideredinthisanalysisduetoinadequatethermalpropertydata.Theresultsofthisanalysisare
showninAppendixA.

Conclusion
Thisexperimentationwasintendedmainlyasacomparisonbetweenvariouscandidateablativematerials.In
thisregardthetestingwasveryuseful,asitdemonstratedmarkeddifferenceinbehaviourbetween
compositions.Furthertestingcanconcentrateonashortlistofviablecandidates.Basedontheir
effectivenessasthermalablativesaswellastheotherdesiredtraits,thetwocandidatesthatcomeoutontop
weretheEpoxy/HydratedMagnesiumSulfateandtheEpoxy/Microspheres.TheBondoGlassandunfilled
Epoxyarealsoworthyofconsideration,theformerduetoitsverylowablationrate,andthelatterduetoits
simplicity.
Whetherornotthesepotentialablativesprovidesufficientthermalprotectiontokeepthepartbeingprotected
belowacertainmaximumtemperaturehasnotbeenaddressedinthisstudy.Theresultsdosuggestthatthis
maywellbethecase,providedsufficientthicknessofablativematerialisused.

AppendixA
THERMCASisathermalanalysissoftwarethatdeterminesthetimevaryingtemperaturedistribution
throughthethicknessofaplate(insulatedornoninsulated)thatresultsfromconvectiveheating,duetohigh
velocitygasflow,overonesurface.
Largelyasanacademicexercise,theexperimentalresultswerecomparedtoTHERMCASpredictedtime
temperaturehistorybasedonassumedthermalpropertiesfortheablativesusedinthisexperiment,andthe
estimatedconvectioncoefficientbasedonheatingofthebarespecimen.
Thedensityandthermalpropertyvaluesforthebasiccomponentsusedintheexperimentalablativesare
showninAppendixB.Thesevalueswerethenusedtoestimatethecorrespondingvaluesfortheablatives
whichconsistedofacombinationofthebasiccomponents.TheresultsareshowninTable2,wherekis
thermalconductivity,Cpisspecificheat,andisthediffusivity,=k/(Cp*density).Densitywas
calculatedbaseduponthemassfractionofeachconsistuent.Thevaluesfortheotherpropertieswere
calculatedusingasimilarmethodology,asafirstorderapproximation.
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Table2DensitiesandthermaldatafortheablativesconsideredintheTHERMCASanalysis
TheresultsoftheTHERMCASanalysiswereplottedtogetherwiththeexperimentallymeasuredvaluesfor
comparison:
EpoxyEpoxy/GlassMicrospheres
Epoxy/Milledglass,50/50Epoxy/Milledglass,30/70
BondoGlass
Inallcases,therewasreasonableagreementbetweentheTHERMCASanalysisandtheexperimentalresults,
consideringtheassumptionsmadeintheanalysis.Notethatitistheslopesofthecurvesthatareofinterest,
whichrepresentthetimerateofchangeoftemperature.Duetothermalinertiaandotherfactors,the
experimentallyobtainedcurveshaveadelayedresponsewithregardtoinitialtemperaturerampup.

AppendixB

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OriginallypostedJuly21,2007

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