纳米材料和纳米结构第十三讲-2-透射电子显微镜及其能谱_精品文档.ppt
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TransmissionElectronMicroscopyandSpectroscopy透射电子显微镜及其能谱,纳米材料和纳米结构,第十三讲,1IntroductiontoTEM,Nanomaterialsaredominatedbyparticleswithsizesinnanometerrange,andthereforetheimagingoftheatomsandthequantitativeanalysisofthesurfacechemistryarevitallyimportantfornanomaterialsresearchTransmissionelectronmicroscopy(TEM)isapowerfulanduniquetechniqueforstructurecharacterization,whichnotonlycanproviderealspaceimagingataresolutionof1-2,butalsoananalyticaltoolforquantitativestructureandchemicalanalysis,
(1)IlluminationSystema.ThermionicEmission;b.FieldEmission
(2)SpecimenStage(3)ObjectiveLensSystem(4)MagnificationSystem(5)DataRecodingSystem(6)ChemicalAnalysisSystema.EnergyDispersiveX-raySpectroscopy(EDS)b.ElectronEnergy-LossSpectroscopy(EELS)c.ChargeCoupledDevice(CCD),InstrumentStructureofTEM,SchematicstructureofaTEM,2AtomicResolutionLatticeImagingofCrystallineSpecimens,QualitiesofTEMimagesaredecidedbythreetypesofcontrast:
DiffractionContrastduetoalocaldistortionintheorientationofthecrystal,whichwillperturbthediffractionintensityandleadstocontrastoftheimagePhaseContrastduetothephasemodulationoftheincidentelectronwave,whichissensitivetotheatomdistributioninthespecimenandisthebasisofhigh-resolutionTEMMassthicknessoratomicnumberproducedcontrastduetoatomswithdifferentatomicnumbersexhibitingdifferentpowersofscattering,2-1ImageContrast,2.2ImagingTheory,2.3ImagingInterpretationandtheoreticalsimulation,TheoreticallysimulatedimagesforadecahedralAuparticalatvariousorientationsandatdifferentfocuses(f=42nmand70nm),3FacetedShapesofNanocrystals,AparticleconstitutingafinitenumberofatomscanhaveaspecificgeometricalshapeSurfaceenergiesassociatedwithdifferentcrystallographicplanesareusuallydifferent,andageneralsequencemayholdforface-centeredcubiccrystal,111100110Forasphericalsinglecrystallineparticle,itssurfacemustcontainhighindexcrystallographyplanes,whichpossiblyresultinalowersurfaceenergyFacetstendtoformontheparticlesurfacetoincreasetheportionofthelowindexplanes,3.1PolyhedralShapesofNanocrystales,Forparticlessmallerthan10-20nm,thesurfaceispolyhedron.Inthefollowingfigure,agroupofcubo-octahedral(立方八面体)shapesasafunctionoftheratio(R)ofthegrowthrateintothatofthearedemonstratedThefastestgrowthdirectioninacube(R=0.58)is,thelongestdirectionintheoctahedron(R=0.7)isthediagonal,andthelongestdirectioninthecubo-octahedronis(R=0.87)isthedirection,Geometricalshapesofcubo-octahedralnanocrystalsasafunctionoftheratio,R,ofthegrowthratealongto,Theparticleswith0.87R1.73havethe111and100facets,theothergroupofparticleshasafixed(111)basewithexposed111and100facets.Anincreaseinthearearatioof111to100resultsintheevolutionofparticleshapesfromatriangle-basedpyramidtoatetrahedron(四面体).,Geometricalshapesofmultiplytwinneddecahedral(十面体)andicosahedral(二十面体)particles,HRTEMimagesofcubicPtnanocrystalsorientedalong(a)001and(b)110,showingsurfacesteps/ledgesandthermodynamicallynonequilibriumshapes,HRTEMimagesofPtnanocrystals(a)withatruncated(去顶的)octahedralshapeandorientedalong110,and(b)withaoctahedralshapeandorientedalong110and001.Theinsetin(a)isamodeloftheparticleshape,HRTEMimagesoftruncatedtetrahedralPtnanocrystalsorientedalong110.Thesurfacestepsandledgesatthetruncatedcornersareclearlyresolved,3.2TwinningStructureandStackingFaults,Twinningisoneofthemostpopularplanardefectsinnanocrystals,anditisfrequentlyobservedforfccstructuredmetallicnanocrystalsTwinningistheresultoftwosubgrainssharingacommoncrystallographicplane,thus,thestructureofonesubgrainisthemirrorreflectionoftheotherbythetwinplaneStackingfaultsaretypicalplanardefect.Theyareproducedbyadistortiononthestackingsequenceofatomplanes,HRTEMimagesof(a)Ptand(b)Aunanocrystalshavingtwin(T)andstackingfault(S)structures,respectively.Thetwinplaneandstackingfaultareparalleltothedirectionoftheelectronbeam,3.3DecahedralandIcosahedralParticles,Thetwomosttypicalexamplesofmultipletwinnedparticlesarethedecahedral(十面体)andicosahedral(二十面体),andthecorrespondingparticlesarethemostextensivelystudiedtwinnednanocrystals.,Atomicmodelsof(a)decahedral,and(b,c)icosahedralnanocrystals,TEMimagesofdecahedralAunanocrystalswhentheincidentelectronbeamisparallelornearlyparalleltothefive-foldsymmetryaxis.Thestrainfieldintroducedbythefive-foldtwinsisapparentin(a).Afouriertransformoftheimageclearlyrevealsthefive-foldsymmetry,3.4NucleationandGrowthofNanoparticles,HRTEMimagesrecordedfromthecentersofcarbonspheres,showingthespiral