第六 七章扫描电子(探针 波谱 能谱仪)

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扫描电子显微分析了解:扫描电子显微镜的结构、工作原理重点:扫描电子显微镜像衬度原理难点:将原理应用到实际样品分析。扫描电子显微术:例子TheeffectofAcceleratingVoltageonSEMImages30kV10kV5kV3kVSpecimen:Toner墨粉Whenhighacceleratingvoltageisusedasat(a),itishardtoobtainthecontrastofthespecimensurfacestructure.Besides,thespecimensurfaceiseasilychargedup.Thesurfacemicrostructuresareeasilyseenat(b).(a)30kVx2,500(b)5kVx2,500Specimen:EvaporatedAuparticles.Theimagesharpnessandresolutionarebetteratthehigheracceleratingvoltage,25kV.(a)5kVx36,000(b)25kVx36,000Specimen:Filterpaper.At5kV,themicrostructuresofthespecimensurfaceareclearlyseenasthepenetrationanddiffusionareaofincidentelectronsisshallow.(a)5kVx1,400(b)25kVx1,400Fig.6Specimen:Sintered(烧结的)powder.Atlowacceleratingvoltage,whilesurfacemicrostructurescanbeobserved,itisdifficulttoobtainsharpmicrographsathighmagnifications.Insuchacase,clearimagescanbeobtainedbyshorteningtheWDorreducingtheelectronprobediameter.(a)5kVx7,200(b)25kVx7,200Specimen:Paintcoat(涂漆).Whenahighacceleratingvoltageisused,morescatteredelectronsareproducedfromtheconstituentsubstanceswithinthespecimen.Thisnotonlyeliminatesthecontrastofsurfacemicrostructures,butproducesadifferentcontrastduetobackscatteredelectronsfromthesubstanceswithinthespecimen.(a)5kVx2,200(b)25kVx2,200SE(secondaryelectron)imaging1.Highresolution(betterthan5nm)isobtainablewithmostSEM’s2.Betterthan2nmresolutionispossibleinsomecases3.10nmresolutionisveryroutine(unlessthesamplelimitstheresolution,asisoftenthecase)Edgeeffect(secondaryelectronemissiondifferingwithsurfacecondition).InfluenceofedgeeffectonimagequalityAmongthecontrastfactorsforsecondaryelectrons,thetilteffectandedgeeffectarebothduetothespecimensurfacemorphology.Secondaryelectronemissionfromthespecimensurfacedependslargelyontheprobe’sincidentangleonthespecimensurface,andthehighertheangle,thelargeremissioniscaused.TheobjectsoftheSEMgenerallyhaveunevensurfaces.Therearemanyslantsalloverthem,whichcontributemosttothecontrastofsecondaryelectronimages.Ontheotherhand,largequantitiesofsecondaryelectronsaregeneratedfromtheprotrusions(突出)andthecircumferences(圆周)ofobjectsonthespecimensurface,causingthemtoappearbrighterthanevenportions.SpecimenIC集成电路chip芯片.Thehighertheacceleratingvoltage,thegreateristheedgeeffect,makingtheedgesbrighter.InfluenceofedgeeffectonimagequalityThedegreeoftheedgeeffectdependsontheacceleratingvoltage.Namely,thelowertheacceleratingvoltage,thesmallerthepenetrationdepthofincidentelectronsintothespecimen.Thisreducesbrightedgeportions,thusresultinginthemicrostructurespresentinthembeingseenmoreclearly.Normally,secondaryelectronimagescontainsomebackscatteredelectronsignals.Therefore,ifthetiltdirectionofthespecimensurfaceandthepositionofthesecondaryelectrondetectoraregeometricallyinagreementwitheachother,morebackscatteredelectronsfromthetiltedportionsaremixed,causingthemtobeseenmorebrightlyduetosynergism合作.(a)5kVx720TiltAngle:50°(b)25kVx720TiltAngle:50°Specimen:ICchip.5kVx1,100Thesidesofpatternsareviewedbytiltingthespecimen.Theamountofsignalsisincreased.Useofspecimentilt:a)Dependenceofimagequalityontiltangle1)Improvingthequalityofsecondaryelectronimages;2)Obtaininginformationdifferentformthatobtainedwhenthespecimenisnottilted,thatis,observingtopographicfeaturesandobservingspecimensides.3)Obtainingstereomicrographs.Fig.13showsaphototakenatatiltangleof0°(a)andaphototakenat45°(b).Theircomparisonshowsthatthelatterisofsmoothqualityandstereoscopicascomparedwiththeformer.Whenthespecimenistilted,howeverlengthsobservedaredifferentfromtheiractualvalues.Whenmeasuringpatternwidths,etc.,therefore,itisnecessarytomeasurewithoutspecimentiltingortocorrectvaluesobtainedformatiltedstate.(a)Tiltangle:0°(b)Tiltangle:45°Specimen:Backsidesofoleaster橄榄leaves.Moreinformationisobtainedfromstereo-pairphotos.Useofspecimentilt:b)Stereo立体micrographsWithSEMimagesitissometimesdifficulttocorrectlyjudgetheirtopographicalfeatures.InsuchacaseobservationofstereoSEMimagesmakesiteasytounderstandthestructureofthespecimen.Besides,stereoobservationallowsunexpectedinformationtobeobtainedevenfromspecimensofsimplestructure.Instereoobservation,afterafieldofinterestisphotographed,thesamefieldisphotographedagainwiththespecimentiltedfrom5ºto15º.Viewingthesetwophotosusingstereoglasseswiththetiltingaxisheldverticallyprovidesastereoimage.Useofspecimentilt:c)DetectorpositionandspecimendirectionTheamountofsecondaryelectronsproducedwhenthespecimenisilluminatedwithanelectronbeam,dependsontheangleofincidencetheoretically.However,therearisesadifferenceintheimagebrightnessdependingonwhetherthetiltedsideofthespecimenisdirectedtothesecondaryelectrondetectorortheoppositeside.Withalongspecimen,forexample,thebrightnessdiffersbetweenthesidefacingthedetectorandtheoppositeside.Insuchacase,directingthelongitudinalaxisofthespecimentothedetectormakesthebrightnessuniform.Fig.16Specimen:FiberDetectorpositionandspecimendirection.Specimen:Fiber7kVx2,200Directingthelongitudinalaxisofthespecimentothesecondaryelectrondetectormakestherightandleftsidesequallybright.(AnSRTunitisusedtodirecttheimagelongitudinally.)Useo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