超分子测试方法总结PPT演示课件

总结,超分子材料分析测试方法,1,现代仪器分析方法,组成分析,结构分析,无机元素分析,有机元素分析,晶体材料分析,有机材料分析,AAS,ICP,有机元素分析仪(CHNOS),XRD,SCD,四大光谱,2,现代仪器分析方法,形貌分析,SEM,TEM,AFM,冷场SEM,W灯丝、LaB6SEM,HRTEM,STEM,FE-SEM,热场SEM,TEM,选取电子衍射像（SAED）高分辨像（晶格条文）形貌像（低倍，高倍）EDS,二次电子像（低倍，高倍）背散射电子像（相貌、组成分析）EDS（谱、点扫、线扫及面扫）,纳米粒子成像表面平整不需喷金,与XPS区别？,3,X射线光电子能谱（XPS，全称为X-rayPhotoelectronSpectroscopy）,定义：是一种基于光电效应的电子能谱，它是利用X射线光子激发出物质表面原子的内层电子，通过对这些电子进行能量分析而获得的一种能谱。,XPS的最大特色：在于能获取丰富的化学信息,对样品表面的损伤最轻微,表面的最基本XPS分析可提供表面存在的所有元素(除H和He外)的定性和定量信息。,正是由于XPS含有化学信息,它也通常被称为化学分析电子能谱（ESCA，全称为ElectronSpectroscopyforChemicalAnalysis），XPS的更高级应用可得到关于表面的化学组成和形成的更详细的信息。,4,XPS，EDS有哪些区别呢?,5,Ag/ZnOheterostructurenanocatalystswithAgcontentof1wt%aresuccessfullypreparedthroughthreedifferentsimplemethods,wherechemicalreductionandphotolysisreactionareadoptedtofabricatetheheterostructure.ThedispersityofAgclustersand/ornanoparticlesinAg/ZnOnanocatalystisinvestigatedbyEDXmappingandXPStechniques.Theexperimentalresultsshowthatdeposition-precipitationisanefficientmethodtosynthesizeAg/ZnOnanocatalystwithhighlydispersedAgclustersand/ornanoparticles;thephotocatalyticactivityofAg/ZnOphotocatalystsmainlydependsonthedispersityofmetallicAginAg/ZnOnanocatalyst;thehigherthedispersityofmetallicAginAg/ZnOnanocatalystis,thehigherthephotocatalyticactivityofAg/ZnOphotocatalystshouldbe.,PhotocatalyticActivityofAg/ZnOHeterostructureNanocatalyst:CorrelationbetweenStructureandProperty,6,PhotocatalyticActivityofAg/ZnOHeterostructureNanocatalyst:CorrelationbetweenStructureandProperty,7,Figure2.Low-magnificationSEMimagesandEDXmappingoftheas-synthesizedsamples:(a)Ag/ZnO-DP,(b)Ag/ZnO-CPand(c)Ag/ZnOST;(d)EDXSspectrarecordedfromthecorrespondingrectangularregionoftheas-synthesizedsamplesina-c.Thecoverageofbluecolorina-creflectsAgdistributionsintheas-synthesizedsamples,andtheinsetinaandcisthecorrespondingHRTEMimageofasingleAg/ZnOheterostructurenanocrystal,8,373.2eV,367.2eV,bulkAgAg3d5/2,368.3eVAg3d3/2,374.3eV,TheshiftofthebindingenergyofmetallicAgindicatesthatthereisastronginteractionbetweenmetallicAgandZnOnanocrystals,AccordingtotheEDXmappingandXPSresults,thisphenomenonshouldbeattributedtothehighestdispersityofmetallicAgonthesurfaceofZnOnanocrystalsforAg/ZnO-DPsample.,Figure3.Ag3dXPSspectraoftheas-synthesizedsamples:(a)Ag/ZnO-DP,(b)Ag/ZnO-CP,and(c)Ag/ZnO-ST.,9,Figure4.(a)UV-visdiffuse-reflectanceand(b)PLspectraoftheas-synthesizedAg/ZnOheterostructurenanocrystals.,Theappearanceoftwokindsofcharacteristicabsorptionbandsalsoconfirmsthattheas-synthesizedsamplesarecomposedofzerovalentAgandZnO.,10,Figure5.PhotodegradationofMObytheas-synthesizedsamples:(a)Ag/ZnO-DP,(b)Ag/ZnO-CP,and(c)Ag/ZnO-ST.Theinsetisthephotographoftheas-synthesizedsamplesdispersedinMOsolution(theconcentrationofthecatalystsis1.25mg/mL).,11,TEMandHRTEMimagesforthegrownZnOnano-needle.,FE-SEMimagesforthenanostructuresgrownonsiliconsubstrate.ZnOgrownfor:(a)30min,(b)60min,(c)180min,and(d)ZnOnano-needlesafterannealingfor180minat500ConlyunderN2atmosphere.,CharacterizationofZnOneedle-shapednanostructuresgrownonNiOcatalyst-coatedSisubstrates,12,TEMimageofanAl2O3-depositedZnOnanorod.Thecentralpart(A)istheZnOnanorodandtheouterpart(B)isthedepositedAl2O3layer.,HRTEMimageofanAl2O3-depositedZnOnanorod.,Al2O3coatingofZnOnanorodsbyatomiclayerdeposition,13,HRTEMimageofananowire.Theleftpartpresentsinterplanarseparationof0.52nmandconsistsofasingleZnOcrystal.Thecrystalgrowthdirection001isperpendiculartotheplanes.ThesmallinclusionsontherightconsistofEr2O3nanocrystals.Theinterplanarseparationof0.30nmcorrespondstothe222direction.,SAEDpatternobtainedatthesurfaceofananowire.Therectangularpatternisduetothe210directioninZnO.TheringsareduetodifferentorientationsofEr2O3nanocryst,StructuralcharacterizationofZnO/Er2O3core/shellnanowires,14,ControlledGrowthandCharacterizationofTungstenOxideNanowiresUsingThermalEvaporationofWO3Powder,SEMimagesofWO3nanowiresgrownontungstensubstrate:(a,b)topviews,(c)tiltview,and(d)EDXspectrumofthenanowiresample,15,Figure3.(a)HRTEMimageofWO3nanowire.Insets(b,c)areenlargementHRTEMsfromsquaresin(a).(d)Diffractionpatternoftungstenoxidenanowires.,Itshowsasinglenanowirewithadiameterof70nmthatexhibitsawell-definedlatticefringeseparationwith0.38nmcorrespondingto001planesofamonoclinicWO3crystal(JCPDSCardNo.75-2072).,16,Figure4.XRDprofileofWO3nanowires.,ThemainpeakscanbewellindexedtobeamonoclinicWO3phase(JCPDSCardNo.75-2072;a)7.274,b)7.501,c)3.824,and)89.930;spacegroupP21/a),whichisingoodagreementwithourTEMandSAEDanalysis.,17,Figure5.XPSprofilesofWO3nanowires.(a)W4fpeaks:thedoublet4f7/2and4f5/2,atbindingenergiesof35.5and37.5eV,respectively,andthetwofitteddoubletsrepresentingthedifferentoxidationstatesofW(greenline,W6+;blueline,W5+)forspecimengrownat1000C.(b)O1speaks:apeakat530.5eVcorrespondingtothevalenceofthetungstenequalto+6andtheotherpeakat532.2eVcorrespondingtoresidualwaterboundinthenanowirestructureoradsorbedonthesurface.,18,Figure6.EvolutionofW4fspectraforthermalannealedWO3nanowiresinthetemperaturerangeof900-1100Cinavacuum.,TheeffectsofthegrowthtemperatureontheoxidationstatesofthetungstenoxidenanowireswerestudiedbyXPS.TheshapeoftheW4fpeakschangesatdifferenttemperatures(Figure6).TheW4fpeakofsamplesannealedat1000-1100CshowsastoichiometricfeatureofWO3.However,forsamplesannealedat900C,thepeakbecomesbroaderandashoulderformsatthehigherbindingenergyside.Thisshouldercorrespondstoloweroxidationstateof2inthexofWOxstructure.Theseresultsindicatethat,athighgrowthtemperatures,WO2readilytransformsintoWO3.,19,Figure7.Ramanspectrumofas-synthesizedprod