Electron Back-Scatter Diffraction in the Scanning Electron Microscope: An Overview

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al! "utline
What is EBSD? Historical Perspective Crystallography & pattern formation Data Collection Recent Developments Conclusions

What is EBSD?
EBSD # electron $ac!scatter %iffraction SE& $ase% techni'ue to measure crystal orientations (pplica$le to any crystalline material )in theory* Provi%es the a$solute crystal orientation +ith su$# micron resolution ( useful tool for %iscriminating $et+een phases

EBSD or EBSP?
EBSD # electron $ac!scatter %iffraction EBSP , electron $ac!scatter %iffraction pattern BKD , Bac!scattere% -i!uchi Diffraction
And some commercial names....

(C)OM , )Crystal* "rientation &apping ACOM , (utomate% Crystal "rientation &apping OIM. # "rientation /maging &icroscopy

al! "utline
What is EBSD? Historical Perspective Crystallography & pattern formation Data Collection Recent Developments Conclusions

EBSD History ,Early Wor!

EBSP li!e patterns +ere first o$serve% $y -i!uchi )0123* in the ransmission Electron &icroscope ) E&*4 5on Boersch )0167* e8ten%e% -i!uchi9s +or!

Mica

EBSD History , (lam et al4

(lam: Blac!man an% Pashley )01;<* use% a cylin%rical specimen cham$er an% film camera to pro%uce high# angle -i!uchi patterns from cleave% =i>: -/: ?aCl: P$S2 crystals4
Lead Sulphide

EBSD History , the $irth of mo%ern EBSD

5ena$les an% Harlan% )0172* o$serve% EBSPs in the Scanning Electron &icroscope )SE&* $y using a 6@mm %iameter fluorescent imaging screen an% a close% circuit television camera4 Dingley )later 013@s* %evelope% the com$ination of phosphor an% television camera: an% com$ine% them +ith a graphical overlay4 EBSP from Dingley's group note calibration marks

EBSD History , continue% e8periments in the 013@s

Commercial soft+are )0131* +as %evelope% to analyse Electron Channeling Patterns )ECP* an% EBSPs4 E& film for high 'uality EBSPs & phase i%entification )013@s*
EBSP from a superalloy collected with EM film

EBSD History , commercial systems in the 011@s

(utomatic metho%s for in%e8ing EBSPs )011@s* an% control of SE&s gave rise to mapping an% phase %iscrimination4 Digital cameras: EDA %ata an% phase %ata$ases provi%e information for phase i%entification )0111 # *

Phase map from duple steel

EBSD History , the present %ay

High spee% mapping $ecomes a reality DualBCross $eam system )Electron C /on $eam* for 6D microscopy Com$ine% chemical an% crystallographic mapping
!rientation map of "i# superalloy$ collected at %&' points ( sec

EBSD set upD

Resulting %iffraction pattern )EBSP*

 Spatial resolutionD %o+n to 0@s of nm Max sample sizeD SE& %epen%ent )typically up to 0@@ 8 ;@mm*

EBSD Performance

Angular resolutionD @42;#0E at present Probe currentD F@42; n( Accelerating voltageD F; !5 Specimen tiltD G@#7;E Working distanceD 0@#<@ mm Speed: @4@0@ # 0 secon% per measurement Sample preparationD electropolishing: colli%al silica polishing : ion $eam milling or etching

al! "utline
What is EBSD? Crystallography & pattern formation Data Collection Recent Developments Conclusions

EBSP crystallography
EBSP symmetry comes from lattice symmetry
, Crystal system: =aue group: space group

o $uil% a crystal
, Start +ith unit cell , (%% a $asis , Repeat a% infinitum444

Huv+I is a crystal %irection: Juv+F is a family of %irections )h!l* is a crystal plane: Kh!lLis a family of planes4

EBSP formation
Electron $eam stri!es specimen Scattering pro%uces electrons travelling in all %irections Electrons that satisfy the Bragg con%ition )nM2%4sin* for a plane )h!l* are channele% -i!uchi $an%s Electrons stri!e the phosphor an% pro%uce light Which is %etecte% $y a CCD camera an% %igitise% he resulting EBSP is automatically analyse% an% in%e8e%444

/ron unit cell

Phosphor

Spherical -i!uchi map

EBSD Resolution
(lthough EBSPs are create% $y $ac!scattere% electrons: the signal %oes not come from the +hole BSE interaction volume /nstea%: the %iffraction signal effectively originates from a Npoint sourceN in the top fe+ nm his means that the EBSD techni'ue can o$tain very high resolutions )J2@nm*

Resolution E8ample 0
Copper interconnect test sample (nalyse% on the =E" Supra ;;5P

Twin domain !"#$" nm wide a%e clea%ly %e ol&ed ' ing a (nm te) i*e

Resolution E8ample 2
Pt thin film (nalyse% on the OE"= G;@@>

=0.08 m; BC; Step=0.005 m; Grid55x49

+%ain with a mean diamete% o, -(nm a%e clea%ly %e ol&ed ' ing a (nm te) i*e

=0.08 m; GB+tri-x; Step=0.005 m; Grid55x49

Bo%y centre% cu$ic /ron {#00} {100}

[001]

(011)
[011] [010]

"

! [100]

{110}

[001] [101] [201] [311] [100] [111] [011]

/ron EBSP
J000F is central ?oteD J000F has 6 fol% symmetry: $ut is close to G fol%4

[210] [110]

[010]

Bo%y an% >ace centre% cu$ic /ron

$cc
Plane Intensity No. K00@L 0@@P 8G K2@@L ;0P 8G K002L 62P 802 K22@L 26P 8G K@06L 07P 802 K222L 06P 8< K026L 0@P 82< Plane Intensity No. K000L 0@@P 8< K2@@L 77P 86 K22@L 63P 8G K006L 2GP 802 K222L 26P 8< K<@@L 0GP 86 K066L 06P 802 K2<@L 02P 802 .cc hC!ClM2n )i4e4 no K000L* ,cc h: !: l all o%% or all even

fcc

Phase %iscrimination
Differences in interplanar angles allo+ similar loo!ing EBSPs from $cc an% fcc /ron to $e %istinguishe%4

$cc /ron
$cc /ron fcc /ron

fcc /ron

al! "utline
What is EBSD? Crystallography & in%e8ing Data Collection Recent Developments Conclusions

/n%e8ing & (utomation

/i&e EBSP 1o'gh )ace

(utomatic analysis
, BeamBStage control

Mo&e .eam o% tage Detect Band

Sa&e data to ,ile Pha e and o%ientation

Inde0 EBSP

A ingle a'tomated EBSD %'n )%o&ide a complete cha%acte%i ation o, the mic%o t%'ct'%e2
Phase %istri$ution e8ture strength Qrain siRe Boun%ary properties &isorientation %ata Slip system activity /ntra#granular %eformation Plus much: much more

all provided !ile you get on it! somet!ing else..."

3o%ked e0am)le o, a'tomated EBSD

(nalysis of polycrystalline samples of halite )?aCl , cu$ic* Some samples have $een e8perimentally %eforme% 5ariations in grain siRe an% in e8tent of su$grain %evelopment necessitate analysis at %ifferent scales
#ata source: $trec!t $niversity% using a P!ilips &'() *+,

Stage can o%ientation ma) o, )olyc%y talline halite

0@@S0@@ gri%: step 0@@ m4

(nalysis timeD <D@< hrs

< mm

Beam can o%ientation ma) o, )olyc%y talline halite

6@@S6@@ gri%: ; m step

(nalysis timeD 6G minutes

;@@ m

EBSD on di,,e%ent cale I

/a%ge a%ea can o, )olyc%y talline halite

64; mm

Compression
Stage scan: 6;@S6@@ gri%: 2; m spacing

EBSD on di,,e%ent cale II

-ie ing intragrain microstructure and local lattice orientation variations... A

2@@ m Reflecte% light image

2@@ m

Beam scan: 2;@S2;@ gri%: 24; m spacing

Absolute and relative misorientation c!anges across transect A./.

G

A
;

A
<

&isorientations relative to 0st %ata point

&isorientation B %egrees

B
0

&isorientations $et+een a%Tacent %ata points

@ @ 0@@ 2@@ 6@@ <@@ ;@@

Distance B microns

EBSD %ata , &aps

P!ase distribution% 0exture% ,rain size 1 s!ape% /oundary properties% Misorientation% Slip system activity% Intra.granular de2ormation....

EBSP 'uality

"rientation fcc

"rientation $cc

Phase map

&isorientation angles for fcc

EBSD %ata , Boun%aries

&isorientation a8is B angle
001

10-15$ (49pt%)

15-#0$ (59pt%)

#0-#5$ (&'pt%)

#5-(0$ (&8pt%)

)*t. +xe% i, r-%t". **rdi,"te% [/0p.ex. pr] 1e-1CC (m(m) C*mp.ete d"t" %et '&90 d"t" p*i,t% 230". +re" pr*4e ti*, 5pper 6emi%p6ere% 1*r!idde, 7*,e .imit%8 0pper ",9.e .*:er ",9.e

111 101

CS= map for fcc

(0-(5$ (1#0pt%)

(5-40$ (#5(pt%)

40-45$ (1'8pt%)

45-50$ (1(#pt%)

50-55$ (#(1pt%)

55-'0$ (5595pt%)

'0-'5$ (#9pt%)
)*t. +xe% i, r-%t". **rdi,"te% [/0p.ex. pr] 1e-1CC (m(m) C*mp.ete d"t" %et '&90 d"t" p*i,t% 230". +re" pr*4e ti*, 5pper 6emi%p6ere% 1*r!idde, 7*,e .imit%8 0pper ",9.e .*:er ",9.e

EBSD %ata , te8ture

OD4

2=0

2=5

2 =1 0

2 =1 5

2 =2 0

2 =2 5

2 =3 0

2 =3 5

2 =4 0

2 =4 5

2 =5 0

2 =5 5

2 =6 0

2 =6 5

2 =7 0
1 1.5 # #.5

2 =7 5

1 =9 0

Pole 4ig'%e
=90 2 =8 0 2 =8 5

al! "utline
What is EBSD? Crystallography & in%e8ing Data Collection Recent Developments Conclusions

Some Recent Developments

04 /mprove% camera technology , increase% sensitivity an% faster %ata ac'uisition 24 Com$ine% EDA an% EBSD , for integrate% mapping an% phase i%entification 64 Use of %ualBcross $eam instruments to o$tain 6D EBSD )com$ine% >/B an% electron $eam*

EBSD %etectors
=o+ light EBSP camera
, Silicon intensifie% target )S/ *
3 $it: very noisy

, CCD , 5 type vi%eo signal

3 $it less noisy

, Slo+ scan CCD

02 $it: lo+ noise: high spee%: $inning

Binning
/ncreases signal: re%uces noise Higher spee% $ut at lo+er resolution

EBSPs # >el%spar

"l% Camera

?e+ Camera

E0am)le O%ientation Ma)

Single Vircon QrainD su$structure% at one e%ge: $ut a single orientation in centre4 20:;<; points: 27 minutes )06 pts B s*

?i#superalloy G@:@@@ points 07 minutes )G6 pts B sec* 16P in%e8ing

Halite # ?aCl 020:2@< points <3 minutes )<2 pts B sec* 16P in%e8ing

6D#EBSD

al! "utline
What is EBSD? Crystallography & in%e8ing Data Collection Recent Developments Conclusions

Conclusions
EBSD is an SE&#$ase% techni'ue that has $een !no+n for ;@ years: $ut only +i%ely applie% in the last 0@ years EBSD is no+ a fast: automate% techni'ue: applica$le to most crystalline materials EBSD provi%es phase i%entification: te8ture an% $oun%ary characteristics44444