分析电镜.pptx

前言前言目的1微观分析结构形貌成分位向原子电子态2实验方法阅读文献内容1.分析型电镜:Scanning-TransmissionElectronMicroscope2.高分辨透射电镜HightResolutionTransmissionElectronMicroscope3.能谱-损失谱ElectronEnergy-lossSpectroscopy4.扫描隧道显微镜ScanningTunnelMicroscope5.原子力显微镜AtomicForceMicroscope6.场离子显微镜FieldIonMicroscope7.三维原子探针3DimensionalAtomProbe8.俄歇谱仪AugerElectronSpectroscopy9.X射线光电子谱仪X-rayElectronSpectroscopy10.背散射电子衍射取向成像ElectronBackScatteringDiffraction11.正电子分析PositronAnnihilateTechnology12.穆斯堡尔谱MssbauerSpectroscopy原理仪器结构应用实例提纲例：例：三维原子探针三维原子探针3DAPm/n=2eVt2/L2参考文献：材料物理现代研究方法材料物理现代研究方法 马如璋马如璋现代分析技术现代分析技术 陆家和陆家和透射电子显微学透射电子显微学 孟庆昌孟庆昌电子显微分析实用方法电子显微分析实用方法 吴杏芳吴杏芳Transmission Electron Microscopy -Applications in Materials Science Xiao-Feng Zhang Electron Microscopy of Nanotubes材料评价的分析电子显微方法材料评价的分析电子显微方法 进藤进藤 大辅大辅材料评价的高分辨电子显微方法材料评价的高分辨电子显微方法 进藤进藤 大辅大辅材料分析测试方法材料分析测试方法 黄新民黄新民高分子物理近代研究方法高分子物理近代研究方法 张俐娜张俐娜近刊论文近刊论文第一章第一章 分析型电子显微镜分析型电子显微镜分析电镜1.STEM方式方式2.衍射（纳米束衍射）衍射（纳米束衍射）3.CBED会聚束衍射会聚束衍射4.EDS分析能谱分析分析能谱分析5.EELS分析损失谱分析（能量过滤）分析损失谱分析（能量过滤）STEM光路图一、STEM模式散射体积能损谱能损谱-能谱空间分辨率比较能谱空间分辨率比较二、衍射和纳米束衍射衍射光路图聚焦束衍射光路图摇摆束上偏转线圈上偏转线圈下偏转线圈下偏转线圈检测器检测器衍射和纳米束衍射的特征选区衍射误差衍射花样标定相同衍射斑点强度变化孪晶和变形三、CBED会聚束衍射CBED形成模式会聚束衍射盘高阶劳厄带HOLZ线会聚束衍射花样HOLZ线高阶劳厄带HOLZ线的形成HOLZ线指数标定1.常规花样常规花样2.小小CBED花样（花样（L=30-50cm）3.000 hkl盘（盘（L=120-300cm）4.标定常规花样标定常规花样5.对比确定衍射盘指数对比确定衍射盘指数HOLZ线分裂测量柏氏矢量不分裂点阵常数测定点阵常数测定（立方系）N=1，2会聚角的测量会聚角的测量测量偏离矢量、消光距离K-M线线测量偏离矢量S和消光距离其它：晶体点群其它：晶体点群萃取复型试样/STEMDeterminationoflatticeparametersfrommultipleCBEDpatterns:AstatisticalapproachUltramicroscopyVolume110,Issue4,Inthefirstpartofthiswork,theobjectivesaretoassesswhatcouldbetheprobabilitydistributionoftherandomerrorsmadeinthelatticeparametermeasurementsfromasingleCBEDpattern,andtogiveanestimateofthesystematicerror.Inthesecondpart,thepossibilityofreducingtherandomerrorbyusingastatisticalapproachforthedeterminationofthelatticeparametersfrommultiplepatternsisconsidered.Tocarryoutthestudyalargenumberofdiffractionpatternswereacquired.Fig.2showsthelocationoftwentydiffractionpatternsusedinouranalysis.Theywereobtainedforalphatiltanglesbetween24and+24fromthesameareaofthesiliconsinglecrystalat93K.Particulartiltanglesandthecorresponding(approximate)zoneaxesarelistedinTable2.Thetableshowsthatnolow-indexzoneaxes(forwhichdynamiceffectsarestronger)wereused.ThisworkisdevotedtotheanalysisoftheuncertaintyinlatticeparametermeasurementsbyCBEDandtomethodsofdecreasingit.Theanalysisofalargenumberofdiffractionpatternsacquiredfromahighpuritysiliconsampleat93KwiththeCBEDtechniqueindicatesthepresenceofbothtypesoferrors:randomandsystematic.Therandomerrorfollowsthenormaldistribution,andtherelativestandarddeviationisabout34104forlatticeparametermeasurementsmadefromonesinglepatternwithaLaB6TEMwithoutenergyfilter.Themainsystematicerrorapparentlycomesfromthedeterminationoftheactualvoltage.Actually,itisarandomerrorwithnormaldistribution.Itappearsasasystematicerroronlybecauseoftheexperimentalprotocolaccordingtowhichthesameactualvoltagevalueisassignedforallpatternsacquiredinasession.Itisshownthatbothrandomandapparentsystematicerrorscanbereducedbyastatisticalapproachbasedonmultiplepatterns.Theaccuracyisabout33.5104usingthree-patternprojectstotheactualvoltagedeterminationandaprecisionofabout1.52104canbereachedusingaminimumofthreepatternsforthedeterminationofthesingle“a”parameterandabout5104forthedeterminationofthecompletesetofLPsforsixdiffractionpatterns.Moreover,theuseofthree(ormore)patternsallowsalsotoovercometheambiguityproblemlinkedtotheCBEDstudy.Themultiple-patternapproachhasthedrawbackofreducingthespatialresolutionduetothedifferenttiltanglesusedfortheacquisitionofthediffractionpatterns.However,forusualstudy,whenonlythreepatternsarenecessary,theeffectofthetilt,whichcanberelativelysmall,isnotdetrimental.Determination of lattice parameters from multiple CBED patterns:A statistical approachOriginalResearchArticleUltramicroscopy,Volume 110,Issue 4,March 2010,Pages 269-277G.Brunetti,E.Bouzy,J.J.Fundenberger,A.Morawiec,A.TiduLattice distortions in GaN on sapphire using the CBEDHOLZ techniqueOriginalResearchArticleUltramicroscopy,Volume 109,Issue 10,September 2009,Pages 1250-1255D.V.SridharaRao,K.McLaughlin,M.J.Kappers,C.J.HumphreysEffect of WC or NbC addition on lattice parameter of surrounding structure in Ti(C0.7N0.3)Ni cermets investigated by TEM/CBEDOriginalResearchArticleJournal of the European Ceramic Society,Volume 30,Issue 10,August 2010,Pages 2131-2138SeongwonKim,Jian-MinZuo,ShinhooKangEffect of sample bending on diffracted intensities observed in CBED patterns of plan view strained samplesOriginalResearchArticleUltramicroscopy,Volume 108,Issue 4,March 2008,Pages 295-301F.Houdellier,D.Jacob,M.J.Casanove,C.Roucau