Characterisation of displacement cascade damage in Cu/sub 3/Au produced by fusion-neutron irradiation

234 Pages·2001·6.79 MB·English

by  C A English Affiliation: UKAEA Atomic Energy Research Establishment, Harwell. Metallurgy Div., M L Jenkins

Characterization of Radiation Damage by
Transmission Electron Microscopy
Series in Microscopy in Materials Science
SeriesEditors: BCantor
MJGoringe
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Series in Microscopy in Materials Science
Characterization of Radiation
Damage by Transmission
Electron Microscopy
M L Jenkins
Department of Materials
University of Oxford, UK
M A Kirk
Materials Science Division
Argonne National Laboratory, USA
Institute of Physics Publishing
Bristol and Philadelphia
c IOPPublishingLtd2001
(cid:13)
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MJGoringe
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Contents
Preface ix
1 The role of transmission electron microscopy in characterizing
radiationdamage 1
1.1 Introduction 1
1.2 Whatisradiationdamage? 1
1.3 Whyiselectronmicroscopyusefulforstudyingradiationdamage? 2
1.4 ThelimitationsofTEM 4
1.5 Thescopeofthebook 4
1.5.1 Organizationofthebook 5
2 Anintroductiontotheavailablecontrastmechanismsand
experimentaltechniques 6
2.1 Diffraction(orstrain)contrast 6
2.1.1 Two-beamdynamicalconditions 7
2.1.2 Bright-fieldkinematicalconditions 9
2.1.3 Down-zoneconditions 11
2.1.4 Weak-beamdark-fieldconditions 11
2.2 Structure-factorcontrast 19
2.3 Phasecontrast 20
2.4 Afewwordsonimagerecording 22
2.5 Commentsonspecimenpreparationandimageartefacts 24
3 Analysis of small centres of strain: the determination of loop
morphologies 27
3.1 Black–whitecontrastanalysis 28
3.1.1 Generalpropertiesofblack–whitecontrastimages 28
3.1.2 Burgersvectordeterminationbylll-vectoranalysis 31
3.1.3 Imagesimulations 33
3.1.4 Examples of image matching to determine Burgers
vectorsandhabit-planes 50
3.1.5 Black–whiteimagesofSFT 55
3.2 Weak-beamimaging 57
3.2.1 Weak-beamanalysesofclustersofsize>5nm 57
v
vi Contents
3.2.2 Weak-beamanalysesofclustersofsize<5nm 69
3.3 Thefutureforsimulationsofdiffractioncontrastimages 70
4 Analysis of small centres of strain: determinationof the vacancyor
interstitialnatureofsmallclusters 74
4.1 Theinside–outsidemethod 74
4.1.1 Edgeloops 75
4.1.2 Non-edgeloops 80
4.1.3 Example:loopsinneutron-irradiatediron 85
4.1.4 Determiningtheloophabit-plane 85
4.2 Theblack–whitestereotechnique 90
4.2.1 Examplesofuseofblack–whitestereoanalysis 93
4.3 The21Dtechnique 100
2
4.4 Determiningthenatureofstacking-faulttetrahedra 102
4.4.1 ThemethodofKojimaetal(1989) 102
4.4.2 ThemethodofCoeneetal(1985) 103
4.5 Indirecttechniquesfornaturedetermination 106
5 Analysisofsmallcentresofstrain:countingandsizingsmallclusters110
5.1 DeterminationofloopandSFTnumberdensities 110
5.1.1 Thereisafiniteresolutionlimit—someloopsarenotseen
becausetheyaretoosmall 110
5.1.2 In any one micrograph, only a proportion of the
resolvableloopswillbeseen 111
5.1.3 Loopsmaybelostfromthefoilduetosurfaceimageforces112
5.1.4 Counting may be difficult if the loop number density is
veryhigh 112
5.1.5 Foil-thicknessmeasurementwill benecessaryif volume
(ratherthanarea)numberdensitiesareneeded 114
5.1.6 For defect yields in irradiation experiments, it is also
necessarytoconsidererrorsindosemeasurement 114
5.2 DeterminingloopandSFTsizes 115
5.2.1 Examplesofimagesizingbyweak-beammicroscopy 122
6 Characterizationofvoidsandbubbles 129
6.1 ‘In-focus’imagingoflargervoids 129
6.2 ‘Out-of-focus’imagingofsmallervoids 130
6.3 Sizingofvoids 132
6.4 Weak-beamimagingofsmallvoids 138
6.5 Over-pressurizedbubbles 138
6.6 Voidarrays 141
7 Techniquesforimagingdisplacementcascades 145
7.1 Imagingdisorderedzonesinorderedalloys 145
7.2 Imagingofamorphouszonesinsemiconductors 154
Contents vii
8 High-resolutionimagingofradiationdamage 159
8.1 Conditionsforstructuralimaging 159
8.1.1 Thespecimen 159
8.1.2 Themicroscope 160
8.2 ImagesimulationsinHREM 161
8.3 ApplicationsofHREMtoradiationdamage 161
8.3.1 Determinationofthenatureofstacking-faulttetrahedrain
silverproducednearlinedislocationsbyelectronirradiation161
8.3.2 Identification of amorphous and recrystallized zones at
cascade sites in the high-temperature superconductor
YBa2Cu3O7−δ 162
8.3.3 Identification of the structure of GeV ion tracks, which
actaspinningdefectsinhigh-temperaturesuperconductors164
8.3.4 Determination of the structure of copper precipitates in
electronandneutronirradiatedFe–Cualloys 168
8.3.5 Determination of the structure of solid Xe precipitates
(‘bubbles’)inelectron-irradiatedaluminium 169
9 Insituirradiationexperiments 173
9.1 Introduction 173
9.2 Insituelectronirradiation 174
9.3 Insituionirradiation 184
9.4 Futurepossibilities 192
10 Applicationsofanalyticaltechniques 194
10.1 Examplesoftheuseofanalyticaltechniquesinradiationdamage 195
10.2 Futuretrends 207
11 Radiationdamageinamorphousglasses 208
11.1 Propertychangescausedbyirradiation 208
11.2 Directionsforfuturework 209
11.3 Variablecoherencemicroscopy(specklepatterns) 211
A TheThompsontetrahedron 214
References 216
Index 222
Wewishtoacknowledgethefollowingforpermissiontoreproducefigures.
AcademicPress: BrownC1976ProceedingsofEMAG75edJAVenebles,
p 405. American Institute of Physics: Allen C W et al 1999 Migration and
coalescence of Xe nanoprecipitates in Al induced by electron irradiation at
300 K Applied Physics Letters 74(18) 2611–13; Maiti A et al 1999 Damage
nucleationandvacancy-inducedstructuraltransformationinSigrainboundaries
AppliedPhysicsLetters75(16)2380–2. AmericanPhysicalSociety: YanYand
Kirk M A 1998 Physical Review B 57 6152; Birtcher R C and Donelley S E
1996 Physical Review Letters 77 4374; Gibson J M and Treacy M M J 1977
Physical Review Letters 78 1074. Blackwell Science: Jenkins M L et al 1973
Journal of Microscopy 98 155, figures A, B, C, D, E, F; Titchmarsh J M and
Dumbill S 1997Journalof Microscopy 188224. ElsevierScience: Howe L M
1980NuclearInstrumentsandMethodsinPhysicsResearch170419;KirkMAet
al2000JournalofNuclearMaterials27650;KiritaniM1994JournalofNuclear
Materials 216 220; Fukushima H 1994 Journal of Nuclear Materials 212–215
154; Jenkins M L 1994Journalof Nuclear Materials 216124; SagaradzeV V
etal1999JournalofNuclearMaterials274287;EnglishCAandJenkinsML
1981JournalofNuclearMaterials96341;HoweLMandRainvilleMH1977
Journalof Nuclear Materials 68 215; KingW E et al 1983Journalof Nuclear
Materials11712; KiritaniMetal 1993JournalofNuclearMaterials 205460;
WilliamsTMetal1982JournalofNuclearMaterials107222;ShepherdCM
1990 Journal of Nuclear Materials 175 170; Titchmarsh J M and Dumbill S
1996 Journal of Nuclear Materials 227 203. Gordon and Breach Publishers:
RuhleMandWilkensM1975RadiationEffectsandDefectsinSolids,SectionB:
Crystal Lattice Defects and Amorphous Materials 6 129. Institute of Physics
Publishing: Eyre B L et al 1977 Journal of Physics F: Metal Physics 7 1359.
OxfordUniversityPress: JenkinsMLetal1999JournalofElectronMicroscopy
48323. TheRoyalSociety: SaldinDKetal1979Phil. Trans. Roy. Soc. Lond.
A292524,figure13;BulloughTJetal1991Proc. Roy. Soc. Lond. A43585;
BlackTJetal1987Proc.Roy.Soc.Lond.A409177,figure1.
Preface
Our motivation for writing this book was two-fold. First, no existing book
providesacompleteanddetaileddescriptionoftheTEMtechniqueswhichhave
beendevelopedforcharacterizationofsmallpoint-defectclustersandotherfine-
scale radiation damage microstructures. Several good books cover the general
theoryandpracticeoftransmissionelectronmicroscopy(e.g.Hirschetal1967,
Williams and Carter 1996), but none describes fully the range of techniques
considered here. These books do of course cover many topics, especially
diffractiontheory,inmoredetailthanispossibleinthisbook.Second,wefearthat
importantlessonsfromthepast,especiallyaboutsomeoftheinherentdifficulties
andlimitationsofsomeofthetechniques,areindangerofbeingforgotten.
We hope for these reasons that this book will be of practical use to
microscopistsworkinginthefieldofradiationdamage.Severalofthetechniques
described should also be useful more generally, in applications where it is
necessarytocharacterizefine-scale,complexmicrostructures. Wewillshow,for
example, some studies of ion-implantation damage in semiconductors and flux
pinningdefectsinsuperconductors.
Weareindebtedtoalargenumberofourfriendsandcolleagueswithwhom
we have workedover the years. We would mentionparticularly Colin English,
Ian Robertson and Hiroshi Fukushima. We are grateful to Ian, Hiroshi, Brian
Eyre, Michio Kiritani, Murray Gibson, Bob Birtcher, Charles Allen, Stephen
Pennycook, Paul Okamoto and Robin Scha¨ublin who all contributed original
micrographs.
Most of our own research and publications in this field comes through
our association with many talented and hard-working graduate students and
postdoctorates over the past 20 years. For this we wish to thank Mike Bench,
TomBlack,TimChandler,TyDaulton,MarcusFrischherz,GrahamHardy,Simon
King, Phil Knight, Bill Lee, Alison Nicol, Peter Othen, Jonathan Perks, Ian
Robertson, Martin Robinson, Barry Shepherd, Brad Storey, Czes Pienkowski,
JohnVetrano,BobWheeler,andYongYan.
Someofthematerial, particularlyinchapters2–5, hasbeenpublishedina
similarforminareviewbyoneoftheauthors(Jenkins1994). Wearegratefulto
ElsevierPressforpermissiontoreproducethismaterialhere. Manyotherfigures
havebeentakenfromtheliterature,andwearegratefultothevariouspublishers
ix
x Preface
forpermissiontousethese.Thesourcesofthefiguresarestatedinfigurecaptions.
Wearealsogratefultoourhomeinstitutions,theDepartmentofMaterialsatthe
University of Oxford and the Materials Science Division at Argonne National
Laboratory, for support in this and past endeavours during our frequentmutual
visits. FundingsupportforMAKhascomeprimarilyfromtheUSDepartmentof
Energy,OfficeofScience.
Finally, wethankourfamilies, especiallyourlong-sufferingwivesFelicity
andStephanie,fortheirencouragementandsupport.
MikeJenkins
MarkKirk
Oxford,May2000