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Refinement
Scott A Speakman
13-4009A
x3-6887
speakman@mit.edu
ScottSpeakman,
ScottSpeakman,
ScottSpeakman,
Atom
Wyckof x
f Site
occ.
La
1a
0.00157 1
6f
0.1993
0.5
0.5
0.0027
ScottSpeakman,
ScottSpeakman,
Instrumental Parameters
background
peak profile parameters
cagliotti parameters u, v, w
pseudo-voigt or other profile parameters
asymmetry correction
anisotropic broadening
ScottSpeakman,
ScottSpeakman,
background functions
manually fit background
polynomial
chebyshev
shifte chebyshev
amorphous sinc function
many others for different programs
ScottSpeakman,
profile functions
vary significantly with programs
almost all programs use Cagglioti U, V, and W
H 2 W V tan U tan 2
HSP uses pseudo-voigt, Pearson VII, Voigt, or pseudo-voigt 3 (FJC
asymmetry)
GSAS uses functions derived more from neutron and synchrotron
beamlines
ScottSpeakman,
go to parameters_calc_pattern.pdf
ScottSpeakman,
ScottSpeakman,
Refinement Strategy
Rietveld methods fit a multivarialbe structure-backgroundprofile model to experimental data
lots of potential for false minima, diverging solutions, etc
need to refine the most important variables first, then add more
until an adequate solution is realized
a correct solution may not result
ScottSpeakman,
scale factor
zero shift or specimen displacement (not both)
linear background
lattice parameters
more background
peak width, w
atom positions
preferred orientation
isotropic temperature factor B
u, v, and other profile parameters
anisotropic temperature factors
ScottSpeakman,
ScottSpeakman,
Additional Files
XRD_Basics_HSP_2006.pdf
large collection of information about X-ray diffraction, instrumentation,
and different techniques
Introduction.pdf
overview of Rietveld
parameters_calc_patterns.pdf
overview of parameters involved in calculating a diffraction pattern
ScottSpeakman,
further reading
Rietveld refinement guidelines, J. Appl.Cryst. 32 (1999) 36-50
R.A. Young (ed), The Rietveld Method, IUCr 1993
V.K. Pecharsky and P.Y. Zavalij, Fundamentals of Powder
Diffraction and Structural Characterization of Materials,
Kluwer Academic 2003.
DL Bish and JE Post (eds), Modern Powder Diffraction, Reviews
in Mineralogy vol 20, Min. Soc. Amer. 1989.
CCP14 website http://www.ccp14.ac.uk/tutorial/tutorial.htm
prism.mit.edu/xray/resources.htm
ScottSpeakman,
Rietveld Programs
Free
GSAS + ExpGUI
Fullprof
Rietica
PSSP (polymers)
Maud (not very good)
PowderCell (mostly for calculating patterns and transforming crystal
structures, limited refinement)
Commercial
PANalytical HighScore Plus
Bruker TOPAS (also an academic)
MDI Jade or Ruby
ScottSpeakman,
Examples
Silicon
LaB6
intermetallic LaNi4.85Sn0.15
ScottSpeakman,
Silicon
Open the datafile in HSP
Add the structure model
insert the structure manually
import (insert) a struture file
usually use the CIF format the ubiquitous standard for crystal
structures
HSP can also import ICSD *.cry files and structures from other
refinement programs
GSAS can import CIF or PowderCell files
ScottSpeakman,
a=5.43 A
Si at 0.125, 0.125, 0.125
ScottSpeakman,
ScottSpeakman,
LaNi4.85Sn0.15
The data was taken from Chapter 6 of Fundamentals of Powder
Diffraction and Structural Characterization of Materials, by
Pecharsky and Zavalij
The structure is a bit more complex that our earlier example,
which allows us to explore more features of HighScore Plus
The data (Ch6_1.raw) is in GSAS format, which can be read into
HighScore Plus
I have also included a CIF file from the ICSD (#104685) with all
the main features of the structure described
ScottSpeakman,
Issue to Consider
How can I work without knowledge of the structure?
Use LeBail or Pawley method to determine lattice parameters
Try indexing and solving the structure using the HighScore Plus tools
You will find that there are 16 possible space groups for this material, but
picking the most common (and simplest) choice, P6/mmm, is the right way to go
ScottSpeakman,