专业课课件计算材料学第七章

第七章常用实验数据分析软件X射线多晶衍射分析（JADE，LABOTEX，POPLA）EBSD数据分析（TSL,CHANNEL)数据处理（ORIGIN,EXCEL）单物相成分定性分析（JADE）

一、打开XRD图谱文件二、对图谱进行处理对XRD图谱进行Kα2去除和图谱的平滑处理三、对图谱进行寻峰根据图谱的实际情况设置寻峰条件，对图谱进行寻峰经过寻峰得出峰的相应参数寻峰后所得的峰参数如图所示，包括峰的位置、晶面间距、强度、半峰宽等四、进行衍射峰的匹配设定峰形匹配参数进行衍射峰匹配经过衍射峰的匹配，得出定性结果，本张衍射图谱所对应样品的物相成分为SiO2。多物相成分的定性分析一、打开衍射图谱二、对图谱进行平滑等处理三、设置寻峰参数进行寻峰经过寻峰得到该图谱的衍射峰数据包括峰位、峰强、半峰宽、晶面间距等。四、根据实际情况设置峰匹配参数并进行峰匹配经过峰匹配后得出定性结果该样品所含的混合相有CaCO3、Al2O3、SiO2RIR值法物相半定量分析

以刚才我们定性分析的多物相混合样品为例，要进行半定量，首先要进行定性分析，在定性分析的基础上，再应用RIR值法进行半定量分析。根据刚才定性的分析结果。该样品所含的物相成分为：CaCO3、Al2O3、SiO2。我们通过数据库查寻，查找这三物相的相应RIR值，然后进行RIR值法半定量原理进行半定量计算，得出结果如图。全谱拟合法物相半定量分析全谱拟合法是应用Rietveld程序对所测图谱进行全谱拟合来进行物相的半定量分析。我们还是以刚才分析的样品为例。一、打开XRD图谱文件二、对图谱进行平滑等处理三、设置寻峰参数进行寻峰经过寻峰得到峰的相应参数四、导入CaCO3、SiO2、Al2O3三物相的结构数据五、设置并调整拟合参数进行多次拟合直至得到最佳拟合结果经过多次拟合得到最佳的拟合结果，拟合结果的好与坏有一系列的评判参数如上图。六、拟合完毕得到各物相的半定量结果全谱拟合法求结晶度一、对样品的衍射图谱进行处理和定性分析从上图我们可以看图该图谱有一明显的非晶衍射峰胞。晶相部分的定性结果为：莫来石与石英。二、加入16%的CaCO3标样进行录谱，所得图谱如下。三、对加入标定的图谱进行处理和Rietveld全谱拟合四、拟合完毕得到结晶相的半定量结果五、根据所加标样实际量重新计算各结晶相及非晶态化合物含量纳米材料晶粒度的计算一、打开XRD图谱文件二、对图谱进行平滑等处理三、选取所要测物相的最佳衍射峰进行峰形拟合计算，求出峰的准确参数。四、根据所求的峰参数及仪器宽化，利用谢乐公式求出晶粒尺寸。衍射线变宽（1）如果样品为退火粉末，则无应变存在，衍射线的宽化完全由晶粒比常规样品的小而产生。这时可用谢乐方程来计算晶粒的大小。

式中Size表示晶块尺寸（nm），K为常数，一般取K=1，λ是X射线的波长(nm)，FW（s）是试样宽化，θ是衍射角。

衍射线变宽（2）如果样品为合金块状样品，本来结晶完整，而且加工过程中无破碎，则线形的宽化完全由微观应变引起。式中Strain表示微观应变，它是应变量对面间距的比值，用百分数表示。衍射线变宽（3）如果样品中同时存在以上两种因素，需要同时计算晶粒尺寸和微观应变。情况就复杂了，因为这两种线形加宽效应也不是简单的机械叠加，而是它们形成的卷积。

由于同时要求出两个未知数，因此靠一条谱线不能完成。一般使用Hall方法：测量二个以上的衍射峰的半高宽FW（s），由于晶块尺寸与晶面指数有关，所以要选择同一方向衍射面，如（111）和（222），或（200）和（400）。以sinθ为横坐标，FW(s)×cosθ为纵坐标作图，用最小二乘法作直线拟合，直线的斜率为微观应变的两倍，直线在纵坐标上的截距即为晶块尺寸的倒数。当应变项为零时该公式变为Scherrer公式。晶粒尺寸和应变曲线的求解：EBSD数据分析（TSL)

理解处理过程：认识菜单的主要功能OIM中晶粒的定义datasets分离Data的噪声消除:取向Orientation:宏观系统定义DistributionFunctions(ODFs)绘制ODFs，PF等微观取向差Misorientation:定义-Orientationvs.Misorientation取向分布函数DistributionFunctions(MDFs)绘制MDFs菜单Therearetwomenusthataccessvirtuallyeverything:创建newpartitions导入dataaspartitions噪声消除cleanupthedataset导出text.angfiles检查统计性结果旋转orientationsofeachpointaboutsampleframe裁剪scansections可实现新建:-Maps-Texturecalculation-Textureplots导出grainIDdataassociatedwitheachpoint检查thepartitionstats&definition改变partition的属性:DecidewhichpointstoincludeDefinea“grain”定义晶粒

OIMdefinesasetofpointstoconstituteagrainif:-Apathexistsbetweenanytwopoints(intheset)suchthatitdoesnottraverseamisorientationanglemorethanaspecifiedtolerance-ThenumberofpointsisgreaterthanaspecifiednumberPointswithaCIlessthanspecifiedareexcludedfromstatistics

Note:PointsthatareexcludedaregivenagrainIDof0(zero)inexportedfiles定义晶粒3degrees15degrees相同颜色代表一个晶粒分割（Partitioning）DatasetsChoosewhichpointstoincludeinanalysisbysettingupselectionformulaUsetoselectbyindividualpointattributesUsetoselectbygrainattributesSelectionformulaisexplicitlywrittenhereGrainCIStandardization:ChangestheCIofallpointswithinagraintobethatofthehighestwithineachgrainMostusefulifaminimumCIcriterionisusedinanalyzingdata(preventslowCIpointswithinagrainfrombeinglost)噪声消除（DataCleanup）NeighborOrient.CorrelationPerformedonallpointsinthedatasetForcleanupleveln:Condition1:Orientationof6-nnearestneighborsisdifferentthancurrentpoint(misorientationangle>chosen)Condition2:Orientationof6-nnearestneighborsisthesameaseachotherIfbothconditionsaremet,thepoint’sorientationischosentobeaneighbor’satrandomRepeatlowcleanuplevels(n=3max)untilnomorepointschangeforbestresultsNeighborPhaseCorrelation-SameasGrainDilationbutinsteadofusingthegrainwithmostnumberofneighboringpoints,thephasewiththemostnumberofneighboringpointsisusedOutputOptions:OverwritecurrentdatasetCreate“cleanedup”datasetasanewdatasetWritethe“cleanedup”datasetdirectlytofileNeighborCICorrelationPerformedonlyonpointswithCIlessthanagivenminimumTheorientationandCIoftheneighborwithhighestCIisassignedtothesepointsUsewhenmajorityofpointsarehighCI,andonlyafewbadpointsexistGrainDilation:ActsonlyonpointsthatdonotbelongtoanygrainasdefinedApointespartofthegrainwiththemostnumberofsurroundingpointsTakestheorientationandCIoftheneighboringpointwithhighestCIUsetoremovebadpointsduetopitsoratG.Bs相邻关系未经噪声消除Level0Level3NotethatHighercleanuplevelsareiterative(i.e.Level3=Levels0,1,2,3)取向（Orientation）的定义Bydefinitionanorientationisalwaysrelative.TheOIMusesthesamplesurfacetodefinetheorthogonalreferenceframe.Quantitiesaretransformedfromsampleframetocrystalframee1se2sj1Fj2NB:amorecomprehensivediscussionofreferenceframesisgivenlater晶粒取向分布函数（OrientationDistributionFunctions）TheODFdisplayshowthemeasuredorientationsaredistributedinorientationspaceTwotypesofdistributionscanbecalculated:DiscreteODF:Binsizedefinesthevolumeofeachelementinorientationspace(5ox5ox5o)FastcalculationSuitableformosttexturestrengthsbutnotweaktexturesifthenumberofgrainsissmall(considerthenumberofdatapointspercellrequiredtoachievereasonablylownoise)ContinuousODF:GeneralizedSphericalHarmonicFunctions:Rankdefinesthe“resolution”ofthefunctionEquivalenttoaFouriertransformCalculationtimerisessteeplywithranknumber(32isaneffectivemaximum)TimeintensiveMostlyappropriateforweakertexturesSomesmoothingisinherent绘制取向分布函数图OnemustselectthetypesofdatavisualizationdesiredPolefiguresshowthedistributionofspecificcrystalplanesw.r.t.samplereferenceframeForthegenerationofmorethanonePF,theyneedtobeaddedoneatatime.InversePoleFiguresareusedtoillustratewhichcrystalplanenormalsareparalleltosampledirections(generallyRD,TD&ND)Theindicesenteredrepresentwhichsamplereferenceframeplaneisbeingconsidered:100,010and001aretypicalchoicesMultipleplanesalsoneedtobeenteredoneatatimeEulerspaceplotshowsthedistributionofintensityasafunctionoftheEuleranglesUsedtovisualizepocketsoftextureaswellas“fiber”texturesResolutiondefineshowmanyslicesarepossibleintheplotODF/PoleFigure/InversePFPlotsChoosetextureanddesiredplottypeUsetoaddmultipleplotstothesameimageSingleEBSDmap(1mm2)Multiplemaps,differentlocations(total=1mm2)RDTDND{100}(001)0.71.42.02.84.05.68.011.3asymmetryofintensityHomogeneity/heterogeneityofthespecimen...equiaxedTiNotjustthenumberofgrainsmustbeconsideredbutalsotheirspatialdistribution:统计性结果Texture–MicrostructureCouplingExample:partialtextureofpopulationsofgrainsidentifiedbyagrainsizecriterion(zirconiumattheendofrecrystallization)partialtextureofthelargestgrainsPartialtextureofthesmallestgrainsImportantfortextureevolutionduringgraingrowth:thelargegrainsgrowattheexpenseofthesmallgrains.Sincethelargegrainshaveadifferenttexture,theoveralltexturealsochangesduringgrowth.D>2D(=11µm)3496grains17.9%surf.D<D/2(=2.75µm)14255grains1.7%surf.Globaltexturej1=0°090060Fj27.4116.011.38.05.64.02.82.01.40.7Misorientation的定义MisorientationisanorientationdefinedwithanothercrystalorientationframeasreferenceinsteadofthesamplereferenceframeThusamisorientationistheaxistransformationfromonepoint(crystalorientation)inthedatasettoanotherpointxzygA-1gBx,y,zaresamplereferenceaxesgAisorientationofdatapointA(referenceorientation)w.r.tsamplereferencegBisorientationofdatapointBw.r.t.samplereferenceMisorientation=gBgA-1Againthefunctioncanbeeitherdiscreteorcontinuous微取向差分布函数（MisorientationDistributionFunctions）CalculatingMDFsisverysimilartocalculatingODFsCorrelatedMDF:MisorientationsarecalculatedonlybetweenneighborsIfthemisorientationisgreaterthanthegraindefinitionangle,thedatapointisincludedThiseffectivelyonlyplotsthemisorientationsbetweenneighboringpointsacrossaG.B.UncorrelatedMDF:MisorientationsarecalculatedbetweenallpairsoforientationsindatasetThisisthe“texturederived”MDFasiteffectivelyiscalculatedfromtheODFOnlyeffectivelyusedifthesamplehasweaktextureTextureReduced:RequiresbothCorrelatedandUncorrelatedMDFstobecalculatedforthesameplottypeThisMDFissimplytheCorrelated/UncorrelatedvaluesMaybeusedtoamplifyanyfeaturesinthecorrelatedMDF绘制MDFsSelecttheTexturedatasetSelecttheplottype(axis/angle;Rodrigues;Euler)UsetogenerateplotsectionsSectionsthroughMisorientationSpace图表Increasingbin#晶界重构（ReconstructedBoundaries）DataMUSTbeonhexagonalgridCleanupthedatatodesiredlevelChooseboundarydeviationlimitGenerateamapwithreconstructedboundariesselectedExportg.b.dataintotextfileThistypeofdataisrequiredforstereologicalanalysisof5-parametergrainboundarycharacterThesoftwareincludesananalysisofgrainboundariesthatoutputstheinformationasa(long)listoflinesegmentdata.useoftheGBsegmentanalysisisanessentialpreliminarystepbeforeperformingthestereological5-parameteranalysisofGBCD.Thedatamustbeonahexagonal/triangulargrid.Ifyouhaveamaponasquaregrid,youmustconvertittoahexagonalgrid.UsethesoftwarecalledOIMToolstodothis(freelyavailablefortranprogram).参考系统（ReferenceFrames）Thisnextsetofslidesisdevotedtoexplaining,asbestwecan,howtorelatefeaturesobservedinEBSDimages/mapstotheEulerangles.Ingeneral,theEulerframeisnotalignedwiththex-yaxesusedtomeasurelocationsinthemaps.TheTSLandChannelsoftwaresbothrotatetheimage180°relativetotheoriginalphysicalsample.BothTLSandChannelsoftwaresusedifferentreferenceframesformeasuringspatiallocationversusthetheEulerangles,whichis,ofcourse,extremelyconfusing.TSLOIM的参考系统-TD

=-yEulerND

=zEuler-RD

=-xEulerZspatialxspatialyspatialSampleReferenceFrameforOrientations/EulerAnglesReferenceFrameforSpatialCoordinatesCrystalReferenceFrame:Rememberthat,toobtaindirectionsandtensorquantitiesinthecrystalframeforeachgrain(startingfromcoordinatesexpressedintheEulerframe),onemustusetheEuleranglestoobtainatransformationmatrix(orequivalent).+xspatialyspatialRD=xEuler

=100sampleTD=yEuler=010sampleImage:

Notethe180°rotation.“+”denotestheOrigin+Physicalspecimen:

MountedintheSEM,thetiltaxis

isparallelto“xspatial”Thepurplelineindicatesadirection,associatedwith,say,ascratch,ortraceofagrainboundaryonthespecimen.Origin软件做图表格(Worksheet)数据表操作数据编辑数据的导入导出数据的转换(运算)数据分析相关菜单：Edit,Column,Analysis,StatisticsOrigin简介主要功能：1、将实验数据自动画成在二维坐标中的图形，有利于对实验趋势的判断；2、在同一幅图中可以画上多条实验曲线，有利对不同的实验数据进行比较研究；3、不同的实验曲线可以选择不同的线型，并且可将实验点用不同的符号表示；4、可对坐标轴名称进行命名，并可进行字体大小及型号的选择；Origin简介5、可将实验数据进行各种不同的回归计算，自动打印出回归方程及各种偏差；6、可将生成的图形以多种形式保存．以便在其他文件中应用；7、可使用多个坐标轴，并可对坐标轴位置、大小进行自由选择。图形处理(Graph)作图(类型选择)图形属性(包括点、线、坐标、图例)数据点的处理(如Read,Mask)曲线的处理曲线分析曲线拟合图层(Layer)与多条曲线的操作相关菜单：Edit,Data,Analysis,ToolsOrigin的工作界面1.标题栏2.菜单栏3.工具栏4.子窗口5.状态栏Origin的工作界面Origin的工作界面工作表窗口图形窗口子窗口工程管理器扩展工具栏的开启方法:selectView:Toolbars

fromthemenubar.子窗口的种类主要有：TheWorksheetWindow工作表窗口TheExcelWorkbookWindowExcel工作表窗口TheGraphWindow图形窗口TheFunctionGraphWindow函数图形窗口TheLayoutPageWindow版面编排窗口注意:每一子窗口都有自己的菜单系统，

只有当该种类的子窗口处在活动状态时，

相关的菜单和菜单项目才会出现。基本操作基本方法1.使用菜单中的相应命令2.使用工具按钮3.右击鼠标，在弹出的快捷菜单中

选相应命令4.选定对象后双击，打开对话框说明：对象不同，右键菜单和对话框不同，有些对象并不是显性的，如整个图形窗口是一种对象。Origin文件的保存Saveaproject

保存工程Saveachildwindowseparatelyasafile

单独将子窗口作为一个文件保存Saveatemplateasafile

保存为模板文件软件安装与启动双击Origin8.exe启动程序软件设置设置保存软件配置、模板的默认目录软件界面简介工具栏文件夹条目列表例如：Book：数据表Graph：图表工作区导入数据导入单个ASCII数据找到实验记录的数据，打开作图选择作图方式，包括曲线、散点图、点线图和柱状图等我们选择散点图定义x轴和y轴即：ColumnA为x