Rietveld Refinement.

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Presentation transcript:

Rietveld Refinement

Why do Reitveld Refinement?

What are the limitations of Rietveld? Phase detection limit of 1-5% Impurity atom determination New/unknown crystal structures Determination of disorder parameter Multiple parameters can have same effect diffraction patterns Equipment (powder vs. single crystal, x-rays vs. neutrons) Garbage in, garbage out! (noisy data, poor quality sample, poor sample prep)

Basic refinement procedure Background Lattice parameters Peak intensities Peak shapes Peak positions Phase fractions Experimental diffraction pattern Starting crystal structure (.cif, ICSD) Refinement program: GSAS, FullProf Assess: Goodness of fit/R factors Impurity phases Peak/background shapes Difference pattern Instrument file (.inst, LaB6 standard)

Some common challenges/problems False minimas Refinement diverges (“blows up”) Which goodness of fit to choose? R vs. Chi sq? Preferred orientation Large amorphous background Incorrect starting crystal structure or lattice parameter Poor quality data!

Resources and links GSAS/EXPGUI: http://www.ncnr.nist.gov/programs/crystallography/software/gsas.html GSAS tutorials: http://www.aps.anl.gov/Xray_Science_Division/Powder_Diffraction_Crystallography/ FullProf: https://www.ill.eu/sites/fullprof/ PowDLL (file conversion): http://users.uoi.gr/nkourkou/powdll/ Lots of info about fitting parameters: http://www.ing.unitn.it/~luttero/laboratoriomateriali/RietveldRefinements.pdf People: Lauryn Baranowski (lbaranow@mines.edu), Lakshmi Krishna (lkrishna@mines.edu)