Let's Do Experiment Using XRD: How to Interpret the

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.

In crystallography, the terms crystal system,

crystalfamily,andlatticesystemeachrefertooneofseveralclassesofspacegroups,lattices,
pointgroups,orcrystals.Informally,twocrystalstendtobeinthesamecrystalsystemifthey
havesimilarsymmetries,thoughtherearemanyexceptionstothis.Spacegroupsandcrystalsare
divided into 7 crystal systems according to their point groups, and into 7 lattice systems
accordingtotheirBravaislattices.Fiveofthecrystalsystemsareessentiallythesameasfiveof
thelatticesystems,butthehexagonalandtrigonalcrystalsystemsdifferfromthehexagonaland
rhombohedrallatticesystems.
Doing experiment using XRD takes some procedural activities to achieve the objectives.
Collecting, analyzing, and interpreting activities should be done by the researchers.
DataCollection
TheintensityofdiffractedXraysiscontinuouslyrecordedasthesampleanddetectorrotate
throughtheirrespectiveangles.Apeakinintensityoccurswhenthemineralcontainslattice
planeswithdspacingsappropriatetodiffractXraysatthatvalueof .Althougheachpeak
consistsoftwoseparatereflections(K1andK2),atsmallvaluesof2 thepeaklocations
overlapwithK2appearingasahumponthesideofK 1.Greaterseparationoccursathigher
valuesof.Typicallythesecombinedpeaksaretreatedasone.The2positionofthediffraction
peakistypicallymeasuredasthecenterofthepeakat80%peakheight.

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.

The crystallographic directions are fictitious

lineslinkingnodes(atoms,ionsormolecules)ofacrystal.Similarly,thecrystallographicplanes
arefictitiousplaneslinkingnodes.Somedirectionsandplaneshaveahigherdensityofnodes;
thesedenseplaneshaveaninfluenceonthebehaviorofthecrystalsuchasopticalproperties,
absorptionandreactivity,surfacetension,anddislocations(plasticdeformation).Forallthese
reasons,itisimportanttodeterminetheplanesandthustohaveanotationsystem.

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.