Maud全谱拟合精修定量教程

Maud2.0定量教程宋党育整理河南理工大学2007-6Email:[e-mail]:0391-3987976QQ:48096753IntroductionHerearetheinstructionstoperformaRietveldquantitativeanalysisonaZrO2/Al2O3powdersampleusingMaud.Version2.03(releasedSeptember12,2005)orhigherisneededforthistutorial.ThespectrumfortheanalysishasbeencollectedusingastandardBragg-BrentanodiffractometerandthedatafileislocatedinthedatasetsandexamplesdirectoryofMaud(theonecreatedbyyouatthefirstrunoftheprogram).Theprocedurewillstartcreatingabasicanalysisfilesettingupthedatafileandthetwophasestoanalyze.Wewillbuildthisanalysisfileintwosteps:1)Step1:loadthedatafile2)Step2:loadandmodifythephasesOncedefinedtheanalysisfile,wewillstarttheanalysisfollowingtwosteps:3)Step3:setupsomevisibleparameters(specifically,theT-PSZcellparameters)4)Step4:refinethespectrumbythewizardThefinalstep(Step5)willshowtheanalysisoutputtotheuser.Thetutorialwillalsoguidetheusertoamoreaccurateandpreciseanalysisifsomeparameterswerenotasexpected.Thetutorialhasbeenaddedbyseveralfigurestohelpthenoviceinfiguringouteasilythebasicproceduretoperformthiskindofanalysis.Step1:loadthedatafile1)StarttheMaudprogramor,ifyouarealreadyin,chooseNewfromtheFilemenutostartanewanalysisandresetall.2)Loadthedatafilealzrc.datfromtheMauddatabasesandexamplesdirectory(theoneMaudaskedforthefirsttimeyourunit).3)Therearethreewaystodoit.Chooseonlyone.a)LocatethefileinyoursystemanddraganddropthefileovertheplotwindowoftheprincipalMaudframe.Whenyouareoverwiththefileyoushouldnoticetheplotpanelborderishighlighted.b)IntheFilemenuchooseLoaddatafile...,navigatetothefilealzrc.datandloadit(Fig1-1).c)(Thisthirdoneistheusualwhenworkingwithmoredatasetsanddatafiles,togetmorecontrolwheretoaddandhowmanydatafilesforeachdatasettohave)SelecttheDataset_xwiththemouseandpresstoolbarbuttonsimilartoaneye(itsaysedittheselectedobjectofthevisiblelistwhenyougowiththemouseoverit).Anewwindowwillappear,selecttheDatafilestabpanelandpresstheBrowse..buttontoloadthedatafile.Locatethealzrc.datfileinthedatabasesandexampledirectoryandloadit.PresstheOKbuttontoclosethedataseteditwindowatend.Fig1-14)AfterloadingthedatafilethemainMaudwindowshouldlooklikethis(youcandragthedividersbetweenthefourpartsofthemainpaneltoadjusttheirsizeasyouprefer)(Fig1-2):5)Youmayzoominthespectrumplotinsomedetailsbyclick,oldanddragthemouseoverthewindowpartyouwanttozoomin.Doubleclickingtheplotresetthezoomtothenormal.Byrightclickingontheplot(CTRL+click,ifyouhaveaone-buttonmouse)youhaveasmallcontextmenuformanualzoomingorgetacoordinatewindow.PressingthePlotoptionsbuttonyougaincontroloversomeplotcharacteristics.6)WedonotneedtomodifytheInstrument(insidethedataset)astheoneloadedbydefaultisaBragg-Brentanowiththecorrectinstrumentalaberrationsforthisdatafile.7)BeforetoproceedwithStep2(loadandmodifythephases)wesavethisanalysisatthepresentstategivingitanewnamesowecanloaditagainifneeded.TocompletethischooseSaveanalysisas...andchoosealocation(betternotinsidethedatabasesandexamplesdirectory)andanameforthefile.Itisadvicedtouseanamewithextension.parsoincertainsystem(MacOSXforexample)canberecognizedasaMaudanalysisfileanddoubleclickingthefile,itwillbeloadedautomaticallyinMaud.Fig1-2Step2:loadandmodifythephases1)SelectthePhasestabPanelinthemainMaudwindow.2)Thereshouldbenophasesinthelist.Ifany,selectitandpresstheremovebuttoninthetoolbar(theonewitharedcross).3)PresstheLoadanobjectfroma(CIF)databaseorfile...buttontoaddanewphase(eachbuttononthetoolbaractsontheselectedlistandorobject/s).Selectthedatabasefilestructures.mdbfromthedatabasesandexamplesfolder.Awindowwillappearwhereyoucanchoosethecorundum(Al2O3)phasefirstfromthevisiblelistbox(Fig2-1).4)RepeattheproceduretoaddthephaseT-PSZfromthesamedatabase.ItisathetetragonalzirconiaCestabilized.Tip:youmayloadbothphasesfromthedatabaseatoncebyselectingboth.Discontinuousselectionispermitted.OnMacOSXyoucanaddmoreselectionsbyholdingdowntheApplebuttonandselectingwhateveryouneedwiththemouseclick.OnWindowsandLunixthereisthesamecounterpartwiththeirspecificbutton-mouseclickprocedure.5)IfyouwishtocheckthephasecharacteristicsforthecorundumorT-PSZyoumayselectthespecificphaseandthenclickontheeditbuttononthetoolbar(theeyeiconbutton).6)Anewwindowwillappearwiththephasecrystallographicandmicrostructuralcharacteristicandmodels.7)Youdon'tneedtodoanythingatthemoment.AtendclosethosewindowswiththeOKbutton(Fig2-2).Fig2-1Fig2-2Step3:setupsomevisibleparameters;specifically,theT-PSZcellparameters1)Wearenowreadytocheckthestartingparametersforthequantitativeanalysis.Themainideaistoguidealittlethestartinganalysistoensuretheleastsquaresalgorithmmayfindasolution.Ingeneralweshouldcheckthatthephasesweloadedarethecorrectonefortheanalysisandinparticularthatthepeaksofthephasesroughlycorrespondtopeaksinthespectrum.2)Firstwecomputethespectrumbasedontheactualparameters.Todothispressthecalculatortoolbarbutton(thetooltipthatitisshownwhenyouleavethemousefewsecondsoveritsaysComputespectraorfromthe'Refinement'menu,clickontheComputespectramenuitem.Theprogramwillcomputeaspectrumwiththeactualvaluesoftheparameters,phasesetc.andthes