EBSD技术简介

OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EBSD技术简介焦汇胜OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009SEM简介OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009SecondaryElectronSecondaryElectronBackscatteredElectronBackscatteredElectronCathodeLuminescenceCathodeLuminescenceAbsorbedCurrentAbsorbedCurrentElectronBeamInducedCurrentElectronBeamInducedCurrent～10nmXX--rayrayIncidentElectronBeamIncidentElectronBeamSecondaryElectronDetectorSecondaryElectronDetector高能电子与样品的相互作用OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009SEM及微区分析OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009FEINano400场发射扫描电镜及HKLEBSP系统Channel5OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EBSD的术语和定义¾ElectronBack-ScatteredPatternElectronBack-ScatteredDiffraction电子背散射衍射技术简称EBSP或EBSD其他的有：BKD，OIM……¾装配在SEM上使用，一种显微表征技术¾通过自动标定背散射衍射花样，测定大块样品表面（通常矩形区域内）的晶体微区取向OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009•基于SEM的一种测量晶体取向的技术•微观组织的可视化和定量化•晶粒尺寸，分布，晶界表征，应变表征•物相鉴别•分布，尺寸，晶体结构•织构OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009与其他微观表征技术的比较•光学金相•样品制备简单•分辨率低•相鉴别•SEM•分辨率高•配合EDS和EBSDEBSD相鉴别相鉴别••导电样品导电样品•TEM•原子级分辨率•样品制备困难•XRD•样品制备简单•相鉴别•无微观组织信息OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EBSD的历史OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009•1928SeishiKikuchi第一次观察到了电子衍射形成的Kikuchi花样。'P'patternofmica(Kikuchi,JapaneseJournalofPhysics,V,2,1928.)'P'patternofcalcite(Kikuchi,JapaneseJournalofPhysics,V,2,1928.)ThankstoRobertSchwarzerfortheimageOxfordInstrumentsTheBusinessofScience®©OxfordInstruments20091990’s-200419902000SchmidtEBSP&foundsHKL1990Schmidt-ECP1986Link/Dingley1986OIM-Adams1993Michael&Goehner-PhaseID1993Dingleyetal-PhaseID1989Dingley&AdamsfoundTSL1994Kriger-LassenetaluseHough1992SchwarzerOrkid/SEM1997SchwarzerOrkid/TEM1993ThermoNoranofferOrkidandPhaseID~2000PriorusingHKLbreaks100p/sbarrier2004ThermoNoransuppliesHKL2003Link/Oxfordlaunchesownproduct?ThermoNoranoffersTSLEDAXacquiresTSL1999HjelenofferscamerasHKLoffersowncameraNordlys2002Oxford2004EDAX/TSL2004DingleyOn-linedeterminationofcrystal...1984OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009TEM菊池图OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009TEM中电子衍射的种类OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009晶面电子衍射菊池线示意图dθλθθ菊池图的形成原理OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EBSD的硬件示意图图像花样相机电子束样品台控制OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EBSD背散射电子衍射系统OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EBSD探头硬件系统OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009•FSDOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009ForescatteredElectrons(FSEorFSD)•前置背散射探头提供取向信息•FSE图像质量的改善：•FSD与样品的相对位置•合适的束流强度OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009FSD探测器的图像输出BSEImage–AtomicNcontrastOC(FSD)Image–channelingcontrastOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009不同晶体取向对应不同的菊池花样，通过分析EBSP花样我们可以反过来推出电子束照射点的晶体学取向(100)(100)(110)(111)简单的标定原理OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009图像处理及菊池带识别采集花样与数据库进行相及取向的比校对并给出标定结果输出相及取向结果EBSD系统的标定过程取点OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009MappingOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009相空间坐标取向信息测量偏差菊池带信息EBSD数据信息OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009HKL与TSL数据的转换OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009TSLOIM输入ctf文件OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EBSD技术、晶体学、材料学基础•解决实际材料问题要有良好的材料学基础或实际经验材料科学问题材料学基础晶体学EBSD技术OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009典型应用晶粒尺寸宏观织构微区织构再结晶/变形分数亚结构应变分析晶界表征CSL晶界相鉴别相分布相变过程失效分析工业领域金属加工航空核工业汽车制造微电子地球科学材料金属，合金金属间化合物陶瓷薄膜地质材料半导体超导体应用领域OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009LowresolutionFSDimageHighresolutionFSDimageEDS/EBSD结合的相分析OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009(Cr,Fe)7C3OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009OrientationmapPhasesmap2μm2μmOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EDSCrcountsmapEDSCcountsmap2μm2μmOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009相分布图OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009•区分马氏体和铁素体OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009焊点相分析实例220XOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009EBSDFSD图像SEMimageEBSDmapOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009PhasemapSiliconAluminumε-Cu3SnCu-SnLeadβ-TinCopperOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009Orientationmap:AllphasesSi,Al,Cu,PbCu-SnSnCu3SnOxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009PolefigurescomparisonSiliconwafer{100}vs.aluminum{111}OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009β-SnPbLargetingraingenerates{110}polesatcenterofcircle取向关系的测定OxfordInstrumentsTheBusinessofScience®©OxfordInstruments2009晶粒尺寸形状分析=25祄;BC+GB+DT+E1-3;Step=0.7祄;Grid200x200=25祄;Map4;Step=0.7祄;Grid200x200晶粒分析OxfordInstrumentsTheBusinessofSc