AdvancedMaterialsAnalysesUsingthePowderDiffractionFile

T.G.Fawcett,F.Needham,C.Crowder,S.Kabekkodu
InternationalCentreforDiffractionData
Newtown,Square,Pennsylvannia,USA

Abstract:ThePowderDiffractionFile(PDF)inRelease2009contains674,139entriesintwomajor
databases.Release2009PDF4+containspredominatelyinorganicmaterialsandhas291,440material
datasetsandPDF4/Organicscontainsorganicandpharmaceuticalmaterialsandhas370,844material
datasets.Thesedatabasesgroweveryyearasnearly50,000materialanalysesarecurrentlybeing
editedandreviewedfromglobalsourcesonanannualbasis.Thisprovidesaconstantsourceofnew
highqualitydata.Thehigherqualityisaresultofrecentadvancesininstrumentationanddataanalysis
software,appliedpriortopublication,aswellasavigorouseditingandstatisticalreviewofcompiled
dataafterpublication,andbeforeinclusioninthePDF.Thesedevelopmentsmeansthatmaterialscan
beidentified,characterizedandanalyzedwithanarrayofnewdataminingtoolsbackedbyanextensive
classifiedandstandardizeddatabase.Thedatabaseitselfcanbedataminedtoprovideinsightsintothe
materialsstateofmatter,crystallinity,solidsolutionbehavior,polymorphcompositionandmultiphase
composition.

Introduction:ThePowderDiffractionFileisthe
significantdatapresentinadiffractionpattern
collaborativeeffortofseveralinternational
suchasphaseidentification,purity,structure,
databaseorganizations.Thecollaboration
quantitativecontent,crystallitesizeand
resultsincomprehensivematerialdatabases
crystallinity.
thatareusedtoidentifyandquantitate

unknownsolidstatematerials.Amajorand
Experimental:Allthedatashowninthis
continuouseffortoftheICDD,ICDDmembers
presentationweremadewiththePDF
andICDDgranteeshasbeentoedit,classifyand
databasesandtheembeddedsoftware
standardizeallthedatafrominternational
containedinthePDF4productline.Similar
sources.Thisenablesthedatabasetobe
data,butwithasmallerinterfacecanbe
analyzedasaninterrelatedcollectionof
producedwithPDF2productsincombination
materialsenablingdataminingandmany
withtheviewingsoftwareDDView.Thedata
differenttypesofanalyses.Thisprovidesglobal
contentandthenumberofsearchanddisplay
researcherswiththecapabilitytoanalyzeallthe
optionsareshowninTable1.

ResultsandDiscussion:Throughcontinued
bibliographiceffortsandaseriesofstrategic
collaborationsthePowderDiffractionfilehas
dramaticallyincreasedinsize(Figure1)overthe
lastdecade.Thisresultsinchangestothebasic
natureofmaterialidentificationasitwas
practicedfrom19401990inthatusersnow

haveapowerfullibraryofmaterialreferences
andtheywillalwaysgetacandidatematch
Table1.SearchanddisplayoptionsforPDF
usingmodernunknownidentificationsoftware.
productsduringthelast5years.
Thechallengeforglobalresearchertodayisto
havesufficientknowledgeandanalysistoolsso

thattheycanchoosethebestandappropriate
solutionfromamongmanycandidates.

Figure1.GrowthofthePowderDiffractionFile

ICDDincooperationwithworldwidesoftware
developershaveproducedaseriesoftoolsfor
dataanalysis.TheICDDhasconvertedalldatain
itsmaterialdatasetstoarelationaldatabase
withJAVAinterfaces.Thematerialdatasets
containdiffractionpatterns,chemical
nomenclature,structureclassifications,
crystallographicdata,physicalpropertiesand
bibliographicinformationwhichnowcanbe
searched,sorted,graphedandplottedinnearly
endlesscombination.Anexampleofamaterial
entryinPDF4+isshowninFigure2additional
analysistoolshavebeendevelopedsothatthe
basicdatacanbeshownasneutron,
synchrotronorelectrondiffraction,spot
patternsorringpatternsaswellaselectron
diffractionbackscatterpatterns.For125,319
entriesinPDF4+thereisalsoacapabilityfor
moleculardrawing,visualizationand
calculationsforbondangles,distancesand
nearestneighboratoms.

Thestandardizationandclassificationeditorial
processesarealsopoweringtoolsbeing
developedbyOEMsandsoftwaredevelopers
suchasRietveldandLeBailrefinements,pattern
fitting,andclusteranalysistools.
Today,veryfewChineselaboratoriesareusing
theseenhancedcapabilitiesofthePDF4
productlinewhichareseeingwidespreadusage
inNorthAmericaandEurope.However,
Chinesescientistsaremajorcontributorsto
theseproductdevelopmentsbothfromdata

submittedbygranteesandpublisheddata
extractedandeditedfromthegloballiterature
includingChinesescientificjournals.

Figure2.Exampleofamaterialdatasetfor
entryPDF000580382.Thereareseveralother
functionsandnesteddisplaydatanotshown.

PDFproductsnowincludethecontributionsof
thousandsofChinesescientists.These
contributionsincludekeyreferencedataon
energymaterials,electronicmaterials,minerals,
andbothnaturalandsynthetic
pharmaceuticals.

Figure3.UnitcellvolumeversusCeriumweight
%forCedopedzirconia.Pre1990data(top)
andallcurrentdata(bottom).

ThedatashowninFigure3demonstratesdata
miningonceriastabilizedzirconiausingdata
parametersstoredinthedatabase.By
comparingtopandbottomgraphsonecansee
thatalargeamountofdatahasbeenentered
intothePDFsince1990.Everypointonthe

graphrepresentsaseparatematerialanalysis.
Cedopedzirconiaisamaterialnowusedina
widevarietyofcommercialapplications
includingfuelcells,cuttingtoolsand
automotivecatalysts.Inthebottomgraphone
canseeclustersofdatathatwerentas
apparentinthetopgraph.Thesecorrespondto
tetragonalandorthorhombicmodificationsof
thestructureusedincommercialapplications.
Ittheanalysisofamoderncatalyticconverter
theresearcherwouldidentifythatthematerial
wasazirconia,butalsoidentifythatthedopant
wasceria,thecrystalsymmetryofthestabilized
zirconiaaseitherorthorhombicortetragonal,
andtheexactconcentrationoftheceriainthe
commercialmaterial.

Examplesofhowtocombinedataminingtools
withenhancedgraphicstocharacterizesolid
solutions,minorandtracephaseidentification
(below10wgt.%),polymorphanalyses,cluster
analysesandnanomaterialanalysesaretoo
extensivetobeshownhere.Howeverawide
rangeofspecificexamplesarepublically
availableforfreedownloadandreviewonthe
websitewww.icdd.com/resources/tutorials.

Conclusion:ThePowderFileisverydynamic
andnewtoolsarebeingcontinuouslyadded
anddevelopedtoenhancematerialsanalysis.