basic powder xrd methods at recx€¦ · basic powder xrd methods at recx . phase identification,...
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Basic Powder XRD methods at RECX
Phase identification, Quantitative Analysis and Lattice parameter refinement
David Wragg University of Oslo
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What can you get from a Powder Diffraction Pattern?
• Peak positions • Peak Intensities
– Phase identification – Quantitative Analysis
(QPA) – Lattice parameter
refinement
• Peak Shapes
– Crystallite size – strain
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2-Theta - Scale9.4 10 11 12 13
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Diffractometer and Data collection • Any diffractometer!
– automated routine instruments are the most common choice
• Bruker D8 Discover in Oslo • Bruker D8 Advance in
Trondheim – Capillary instruments
may be used to reduce preferred orientation
– More complicated applications require better data
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How Can We Help You?
• Data collection – And advice on data collection methods for specific
samples – We have experience of a range of difficult sample
types
• Training • Phase identification and analysis
– Subject to “man hour” costs
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Phase Identification • Diffraction pattern is a unique fingerprint of the crystal
lattice which produced it • Phases from a database are matched to the observed
pattern using line position and intensity • Sample height correction is important
– Back loading sample holders can help – Capillaries give best reproducibility
• ICDD and COD databases available at both RECX PXRD nodes
• Databases are integrated into the EVA pattern analysis software for automatic searching
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Quantitative Analysis
• The peak intensities are related to the weight fractions of phases in a mixture
• Once the phases in a sample are known they can be quantified
• Traditional method: – Identify unique, non-overlapping peaks for each
phase – measure the intensities – Calculate phase fractions
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Quantitative Analysis
• Modern Method – Full profile Rietveld refinement
• Advantages – More accurate- uses all peaks – Easy to do with modern software and can be automated – Unknown phases can be included (PONKCS method)
• Requirements – Need structural data for the phases (unless using PONKCS) – Need to use Rietveld software (relatively straightforward
today) – Preferred orientation should be avoided
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QPA demo
• Si and LaB6
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Lattice refinement • Substitution of atoms in a lattice changes peak positions and
intensities • We can study the degree of substitution by studying the size of the
crystal lattice (from peak positions) • A starting “parent” unit cell is required • Least squares fitting methods are used
– Old: • Get parent and substituted peak positions • Fit numerically
– New • Fit parent unit cell against substituted data with full pattern refinement • Full Rietveld method (peak intensities from structure) or Structureless
methods (dummy intensities) can be used (Pawley and Le Bail methods)
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Structureless Lattice Refinement Demo
• Co in LiFePO4
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Example Data From Lattice Parameter Refinement
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Ionic Radii Fe2+ = 78 pm Co2+ = 74 pm Data: Ingunn Sandberg Masters Project, 2014
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Summary
• A lot of data can be extracted from quick, routine powder XRD data collections – Phase identification – Quantitative analysis – Lattice parameters – Crystallite size (approximate)
RECX can help you to do this!
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