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Aberration-corrected Analytical Electron Microscopy (RMS - Royal Microscopical Society) PDF

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Aberration-Corrected Analytical Transmission Electron Microscopy Currentandfuturetitles intheRMS-WileyImprint Published Principles and Practice of Variable Pressure/Environmental Scanning ElectronMicroscopy(VP-ESEM) – DebbieStokes Aberration-Corrected Analytical Electron Microscopy – Edited by Rik Brydson Forthcoming UnderstandingPracticalLightMicroscopy – JeremySanderson AtlasofImagesandSpectraforElectronMicroscopists – EditedbyUrsel Bangert Diagnostic Electron Microscopy – A Practical Guide to Tissue Prepa- ration and Interpretation – Edited by John Stirling, Alan Curry & BrianEyden PracticalAtomicForceMicroscopy – EditedbyCharlesClifford Low Voltage Electron Microscopy – Principles and Applications– EditedbyNatashaErdman&DavidBell Focused Ion Beam Instrumentation: Techniques and Applications– DudleyFinch&AlexanderBuxbaum Aberration-Corrected Analytical Transmission Electron Microscopy Edited by Rik Brydson Published in association with the Royal Microscopical Society Series Editor: Susan Brooks A John Wiley & Sons, Ltd., Publication Thiseditionfirstpublished2011 ©2011JohnWiley&Sons,Ltd. Registeredoffice JohnWiley&SonsLtd.,TheAtrium,SouthernGate,Chichester,WestSussex,PO198SQ,UnitedKingdom Fordetailsofourglobaleditorialoffices,forcustomerservicesandforinformationabouthowtoapplyfor permissiontoreusethecopyrightmaterialinthisbookpleaseseeourwebsiteatwww.wiley.com. Therightsoftheauthortobeidentifiedastheauthorofthisworkhasbeenassertedinaccordancewiththe Copyright,DesignsandPatentsAct1988. Allrightsreserved.Nopartofthispublicationmaybereproduced,storedinaretrievalsystem,or transmitted,inanyformorbyanymeans,electronic,mechanical,photocopying,recordingorotherwise, exceptaspermittedbytheUKCopyright,DesignsandPatentsAct1988,withoutthepriorpermissionof thepublisher. Wileyalsopublishesitsbooksinavarietyofelectronicformats.Somecontentthatappearsinprintmay notbeavailableinelectronicbooks. Designationsusedbycompaniestodistinguishtheirproductsareoftenclaimedastrademarks.Allbrand namesandproductnamesusedinthisbookaretradenames,servicemarks,trademarksorregistered trademarksoftheirrespectiveowners.Thepublisherisnotassociatedwithanyproductorvendor mentionedinthisbook.Thispublicationisdesignedtoprovideaccurateandauthoritativeinformationin regardtothesubjectmattercovered.Itissoldontheunderstandingthatthepublisherisnotengagedin renderingprofessionalservices.Ifprofessionaladviceorotherexpertassistanceisrequired,theservicesofa competentprofessionalshouldbesought. Thepublisherandtheauthormakenorepresentationsorwarrantieswithrespecttotheaccuracyor completenessofthecontentsofthisworkandspecificallydisclaimallwarranties,includingwithout limitationanyimpliedwarrantiesoffitnessforaparticularpurpose.Thisworkissoldwiththe understandingthatthepublisherisnotengagedinrenderingprofessionalservices.Theadviceandstrategies containedhereinmaynotbesuitableforeverysituation.Inviewofongoingresearch,equipment modifications,changesingovernmentalregulations,andtheconstantflowofinformationrelatingtothe useofexperimentalreagents,equipment,anddevices,thereaderisurgedtoreviewandevaluatethe informationprovidedinthepackageinsertorinstructionsforeachchemical,pieceofequipment,reagent, ordevicefor,amongotherthings,anychangesintheinstructionsorindicationofusageandforadded warningsandprecautions.ThefactthatanorganizationorWebsiteisreferredtointhisworkasacitation and/orapotentialsourceoffurtherinformationdoesnotmeanthattheauthororthepublisherendorses theinformationtheorganizationorWebsitemayprovideorrecommendationsitmaymake.Further, readersshouldbeawarethatInternetWebsiteslistedinthisworkmayhavechangedordisappeared betweenwhenthisworkwaswrittenandwhenitisread.Nowarrantymaybecreatedorextendedbyany promotionalstatementsforthiswork.Neitherthepublishernortheauthorshallbeliableforanydamages arisingherefrom. LibraryofCongressCataloging-in-PublicationData Aberration-correctedanalyticaltransmissionelectronmicroscopy/editedbyRikBrydson...[etal.]. p.cm. Includesbibliographicalreferencesandindex. ISBN978-0-470-51851-9(hardback) 1.Transmissionelectronmicroscopy.2.Aberration.3.Achromatism.I.Brydson,Rik. QH212.T7A242011 (cid:2) 502.825–dc23 2011019731 AcataloguerecordforthisbookisavailablefromtheBritishLibrary. PrintISBN:978-0470-518519(H/B) ePDFISBN978-1119-978855 oBookISBN:978-111-9978848 ePubISBN:978-1119-979906 MobiISBN:978-1119-979913 Setin10.5/13ptSabonbyLaserwordsPrivateLimited,Chennai,India Contents ListofContributors xi Preface xiii 1 GeneralIntroductiontoTransmissionElectronMicroscopy (TEM) 1 PeterGoodhew 1.1 WhatTEMOffers 1 1.2 ElectronScattering 3 1.2.1 ElasticScattering 7 1.2.2 Inelastic Scattering 8 1.3 SignalswhichcouldbeCollected 10 1.4 ImageComputing 12 1.4.1 ImageProcessing 12 1.4.2 ImageSimulation 13 1.5 RequirementsofaSpecimen 14 1.6 STEMVersusCTEM 17 1.7 TwoDimensionalandThreeDimensionalInformation 17 2 IntroductiontoElectronOptics 21 GordonTatlock 2.1 RevisionofMicroscopywithVisibleLightandElectrons 21 2.2 FresnelandFraunhoferDiffraction 22 2.3 ImageResolution 23 2.4 ElectronLenses 25 2.4.1 Electron Trajectories 26 2.4.2 Aberrations 27 2.5 ElectronSources 30 2.6 ProbeFormingOptics andApertures 32 2.7 SEM,TEMandSTEM 33 vi CONTENTS 3 DevelopmentofSTEM 39 L.M.Brown 3.1 Introduction:StructuralandAnalyticalInformationin ElectronMicroscopy 39 3.2 TheCreweRevolution:HowSTEMSolves the InformationProblem 41 3.3 ElectronOpticalSimplicity ofSTEM 42 3.4 TheSignalFreedomofSTEM 45 3.4.1 Bright-Field Detector (PhaseContrast, Diffraction Contrast) 45 3.4.2 ADF,HAADF 45 3.4.3 Nanodiffraction 46 3.4.4 EELS 47 3.4.5 EDX 47 3.4.6 OtherTechniques 48 3.5 BeamDamageandBeamWriting 48 3.6 CorrectionofSpherical Aberration 49 3.7 WhatdoestheFutureHold? 51 4 LensAberrations:DiagnosisandCorrection 55 AndrewBleloch andQuentinRamasse 4.1 Introduction 55 4.2 GeometricLensAberrations andTheirClassification 59 4.3 SphericalAberration-Correctors 66 4.3.1 Quadrupole-Octupole Corrector 69 4.3.2 Hexapole Corrector 70 4.3.3 ParasiticAberrations 72 4.4 GettingAroundChromaticAberrations 74 4.5 DiagnosingLensAberrations 75 4.5.1 Image-based Methods 77 4.5.2 Ronchigram-based Methods 80 4.5.3 Precision Needed 85 4.6 FifthOrderAberration-Correction 85 4.7 Conclusions 86 5 TheoryandSimulations ofSTEMImaging 89 PeterD.Nellist 5.1 Introduction 89 5.2 Z-ContrastImagingofSingleAtoms 90 CONTENTS vii 5.3 STEMImagingOfCrystalline Materials 92 5.3.1 Bright-field ImagingandPhaseContrast 93 5.3.2 AnnularDark-fieldImaging 96 5.4 IncoherentImagingwithDynamicalScattering 101 5.5 ThermalDiffuseScattering 103 5.5.1 ApproximationsforPhononScattering 104 5.6 MethodsofSimulation forADFImaging 106 5.6.1 AbsorptivePotentials 106 5.6.2 Frozen PhononApproach 107 5.7 Conclusions 108 6 Details ofSTEM 111 AlanCraven 6.1 SignaltoNoiseRatioandSomeofitsImplications 112 6.2 TheRelationshipsBetweenProbeSize, ProbeCurrentandProbeAngle 113 6.2.1 TheGeometricModelRevisited 113 6.2.2 TheMinimumProbeSize,theOptimum AngleandtheProbeCurrent 115 6.2.3 TheProbeCurrent 115 6.2.4 ASimpleApproximationtoWaveOptical ProbeSize 117 6.2.5 TheEffectofChromaticAberration 117 6.2.6 Choosingα inPractice 118 opt 6.2.7 TheEffectofMakingaSmallError intheChoiceofα 119 opt 6.2.8 TheEffectofα OntheDiffraction Pattern 120 6.2.9 ProbeSpreadingandDepthofField 122 6.3 TheCondenserSystem 124 6.4 TheScanningSystem 126 6.4.1 Principles oftheScanningSystem 126 6.4.2 Implementation oftheScanningSystem 128 6.4.3 Deviations oftheScanningSystemFromIdeality 128 6.4.4 TheRelationship BetweenPixelSize andProbeSize 130 6.4.5 Drift,DriftCorrectionandSmartAcquisition 131 6.5 TheSpecimen Stage 133 6.6 Post-Specimen Optics 135 6.7 BeamBlanking 136 6.8 Detectors 137 6.8.1 BasicPropertiesofaDetector 137 viii CONTENTS 6.8.2 Single andArrayDetectors 139 6.8.3 Scintillator/Photomultiplier Detector 139 6.8.4 Semiconductor Detectors 141 6.8.5 CCDCameras 142 6.9 ImagingUsingTransmittedElectrons 145 6.9.1 TheDiffraction Pattern 145 6.9.2 CoherentEffectsintheDiffractionPattern 147 6.9.3 SmallAngularRange – BrightField andTilted DarkFieldImages 152 6.9.4 MediumAngularRange – MAADF 152 6.9.5 High AngularRange – HAADF 153 6.9.6 ConfiguredDetectors 153 6.10SignalAcquisition 154 Acknowledgements 159 7 ElectronEnergyLossSpectrometryandEnergy DispersiveX-rayAnalysis 163 RikBrydsonandNicoleHondow 7.1 WhatisEELSandEDX? 164 7.1.1 BasicsofEDX 164 7.1.2 BasicsofEELS 166 7.1.3 CommonFeaturesForAnalytical Spectrometries 168 7.2 AnalyticalSpectrometries intheEnvironmentofthe ElectronMicroscope 170 7.2.1 InstrumentationforEDX 170 7.2.2 EELSInstrumentation 174 7.2.3 MicroscopeInstrumentationforAnalytical Spectroscopies 178 7.3 ElementalAnalysisandQuantification UsingEDX 182 7.4 LowLossEELS – Plasmons,IBTransitions andBandGaps 187 7.5 CoreLossEELS 191 7.5.1 ElementalQuantification 191 7.5.2 Near-EdgeFineStructureForChemical and BondingAnalysis 195 7.5.3 Extended-EdgeFineStructureForBonding Analysis 200 7.6 EDXandEELSSpectralModelling 201 7.6.1 TotalSpectrumModelling 201 CONTENTS ix 7.6.2 EELSModellingofNearEdgeStructuresand alsotheLowLoss 201 7.7 SpectrumImaging:EDXandEELS 202 7.8 UltimateSpatialResolutionofEELS 206 7.9 Conclusion 207 8 Applications ofAberration-CorrectedScanning TransmissionElectronMicroscopy 211 MervynD.Shannon 8.1 Introduction 211 8.2 SampleCondition 212 8.3 HAADFImaging 213 8.3.1 ImagingofIsolatedAtoms 213 8.3.2 LineDefects (1-D) 219 8.3.3 Interfaces andExtendedDefects(2-D) 220 8.3.4 Detailed ParticleStructures(3-D) 226 8.3.5 Low-lossEELS 230 8.3.6 Core-lossEELSandAtomic-scale Spectroscopic Imaging 231 8.4 Conclusions 236 9 Aberration-Corrected ImaginginCTEM 241 SarahJ.HaighandAngusI.Kirkland 9.1 Introduction 241 9.2 OpticsandInstrumentationforAberration- CorrectedCTEM 243 9.2.1 Aberration-Correctors 243 9.2.2 Related InstrumentalDevelopments 243 9.3 CTEMImagingTheory 244 9.3.1 CTEMImageFormation 244 9.3.2 TheWaveAberrationFunction 246 9.3.3 PartialCoherence 252 9.4 CorrectedImagingConditions 253 9.4.1 TheUseofNegative SphericalAberration 254 9.4.2 AmplitudeContrastImaging 256 9.5 AberrationMeasurement 256 9.5.1 AberrationMeasurementFromImageShifts 256 9.5.2 AberrationMeasurementfrom Diffractograms 257 x CONTENTS 9.5.3 AnAlternativeApproachtoAberration Measurement 258 9.6 IndirectAberrationCompensation 258 9.7 AdvantagesofAberration-Correction forCTEM 259 9.8 Conclusions 259 Acknowledgements 260 AppendixA: AberrationNotation 263 AppendixB: GeneralNotation 267 Index 275

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