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Diffractogram
Basically, XRD (XRay Powder Diffraction), as a nondestructive technique has some
functions for identifying crystalline phases and orientation, determining structural properties
(latticeparameters,strain,grain size,phase composition, thermalexpansion, etc), measuring
thicknessofthinfilmsandmultilayers,determiningatomicarrangement.Thus,XRDismost
widely used for the identification of unknown crystalline materials (e.g. minerals, inorganic
compounds).Determinationofunknownsolidsiscriticaltostudiesingeology,environmental
science,materialscience,engineeringandbiology.
DataReduction
Resultsarecommonlypresentedaspeakpositionsat2andXraycounts(intensity)inthe
formofatableoranxyplot(shownabove).Intensity(I)iseitherreportedaspeakheight
intensity,thatintensityabovebackground,orasintegratedintensity,theareaunderthepeak.The
relativeintensityisrecordedastheratioofthepeakintensitytothatofthemostintensepeak
(relativeintensity=I/I1x100).
DeterminationofanUnknown
Thedspacing of each peak is then obtained by solution of the Bragg equation for the
appropriate value of . Once alldspacings have been determined, automated search/match
routinescomparethedsoftheunknowntothoseofknownmaterials.Becauseeachmineralhasa
uniquesetofdspacings,matchingthesedspacingsprovidesanidentificationoftheunknown
sample.Asystematicprocedureisusedbyorderingthedspacingsintermsoftheirintensity
beginningwiththemostintensepeak.Filesofdspacingsforhundredsofthousandsofinorganic
compounds are available from the International Centre for Diffraction Data as the Powder
DiffractionFile(PDF).ManyothersitescontaindspacingsofmineralssuchastheAmerican
Mineralogist
Crystal
Structure
Database.
DeterminationofUnitCellDimensions
Fordeterminationofunitcellparameters,eachreflectionmustbeindexedtoaspecifichkl
knownasMillerindices.Millerindicesisanotationsystemincrystallographicforplanesand
directionincrystal(Bravais)lattices.Theyarewritten(hkl),andeachindexdenotesaplane
orthogonaltoadirection(h,k,l)inthebasisofthereciprocallatticevectors.Byconvention,
negativeintegersarewrittenwithabar,asin3for3.Theintegersareusuallywritteninlowest
terms, i.e. their greatest common divisor should be 1. Miller index 100 represents a plane
orthogonaltodirection;index010representsaplaneorthogonaltodirectionm,andindex001
representsaplaneorthogonalton.
Assummary,inordertodophaseidentification,oneofthemostimportantusesofXRD,
there are several steps. We can conclude as obtaining XRD pattern, measuringdspacings,
obtaining integrated intensities,and comparing data with knownstandards in the ICDD file
formerlyknownasJCPDS.Inthelaststep,wecanuseJCPDSCard.Thecardcontainfile
number (1), three strongest lines (2), lowest angle line (3), chemical formula (4), data on
diffraction method used (5), crystallographic data (6), optical and other data (7), data on
specimen (8), and data on diffraction pattern (9). Commonly this information is an integral
portionofthesoftwarethatcomeswiththeinstrumentation.