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XRPD_tutorial.exe
Dr Carlo Meneghini
Dip. Di Fisica, Università di Roma Tre
meneghini@fis.uniroma3.it II African School on X-ray in materials
19-24 Jan. 2009
Bibliography
Pwder diffraction: technique and data analysis
• B.E. Warren, X-Ray Diffraction (Addison-Wesley, 1990).
• H.P. Klug and L.E. Alexander, X-Ray Diffraction Procedures (Wiley Interscience, 1974).
• B.D. Cullity, Elements of X-Ray Diffraction (Wiley, 1978).
• Modern Powder Diffraction Reviews in Mineralogy, Volume 20 D.L. Bish and J.E. Post, Editors Mineralogical
Society of America, 1989.
• Fundamentals of Crystallography IUCr Texts on Crystallography -2 C. Giacovazzo, Editor Oxford Science
Publication, 1992.
• The Rietveld Method IUCr Monographs on Crystallography - 5 R.A. Young, Editor Oxford Science Publication,
1993.
• X-ray Diffraction Procedures for Polycrystalline and Amorphous Materials H.P Klug and L.E. Alexander
Wiley-Interscience, 1974, 2nd edition.
• Defects and Microstructure Analysis by Diffraction R.L. Snyder, J. Fiala and H.J. Bunge, IUCr Monographs on
Crystallography, Vol 10, Oxford Science Publications, 1999.
On line resources
http://epswww.unm.edu/xrd/resources.htm A resource page for XRD
http://www.ccp14.ac.uk/ The collaborative computational projects
Peak shapes
Peak relative
intensities
Background Atomic
Peak distribution in
positions the unit cell
10 20 30 40
2θ
XRD_tutorial folder
Data
Programs Analysis
expand
gnuplot
wgnuplot.exe
XRPD experiment done!
Firstly: get a look to the data! More information on
Gnuplot at:
www.gnuplot.info
25000
'y2o3.dat' u 1:2
20000
15000
.../data 10000
5000
plo_y2O3.plt
0
0 20 40 60 80 100 120
Can you
distinguish
Is the statistics good
different peaks?
enough also for weaker
Are the
peaks?
resolution, the
angular step, etc...
appropriate?
If the patterns are good...
...go ahead
If not...
http://database.iem.ac.ru/mincryst/
http://webmineral.com/
http://barns.ill.fr/
http://database.iem.ac.ru/mincryst/
y2o3.dat
ICSD public version
http://barns.ill.fr
00 Our data 'y2o3.dat' u 1:2
00
They reasonably
y2o3.dat
00
match!
00
00
0
10 20 30 40 50 60
database
go ahead!
Literature Data
Go deeper into the data
icsd_86815.cel
PCW
XRD_tutorial folder
PCW
http://users.omskreg.ru/~kolosov/bam/a_v/v_1/powder/details/pcwindex.htm
generate the
pattern
Play with the structure
pattern
look at the whole cell
refinement
Modify/Create the unit cell
diffracted
incoming
beam
beam θ
θ
SNLS – XRPD tutorial/dati
y2o3.x_y
particle size,
Structure stress-strain,
Symmetry texture
Atomic positions,
Experimental site occupancy +
Geometry & thermal Experimental
set-up factors resolution
diffracted
incoming
beam
beam 2θ
displacement
Sample
zeroshift
hkl hkl hkl hkl
icsd_86815
¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯
scaling : 1.2000 1.2000
lattice a: 10.5968 10.6090
overall B : 0.0000 -
global parameters
¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯¯
zero shift : -0.1475 -0.1997
displacement : 0.0000 -
backgr. polynom : 13 13
CMPR
XRPD tutorial
Install CMPR
program on the PC
(defaults options)
http://www.ncnr.nist.gov/xtal/software/cmpr/
Windows installation
http://www.ncnr.nist.gov/xtal/software/cmpr/#WIN
1
To Select diffraction peaks
1) position the mouse at the peak
maximum and
2) pres the p key
Check box to refine or
fix the parameters
GSAS
XRPD tutorial
Make a new
(XP)gsas+expgui.exe
directory in the
path:
C:\gsas\MyWork
Choose a file
name for your
experiment
Use the
icsd_86815.cel
file
hkl hkl hkl hkl
peak breadth Gaussian: σ2 = GU tan2θ + GV tan θ + GW tan2 q + GP/cos2 θ
Gaussian
sample shift: s = - π R shft / 3600 Sherrer
broadening
sample absorption: µeff = - 9000 / (π R Asym)
peak breadth Lorentzian : γ = (LX - ptec cos φ)/cos θ + (LY - stec cos φ) tan θ
Lorentzian Breadth: γ = (LX - ptec cos φ)/cos θ + (LY - stec cos φ) tan θ
Strain: S = ∆d/d
Gaussian contrib. S = sqrt[8 ln 2 (GU- Ui)] (π/18000) · 100%
Instrumental
contribution
Particle size: P
P = (18000/ π) K λ / LX
Scherrer
constant
2 1 4 3
Mp = Σ w (Iexp-Icalc)2
Rp = Σ (Iexp-Icalc) / Σ Iexp
χ2 = Mp / (Nobs - Nvar )
GSAS
SNLS – XRPD tutorial
(XP)gsas+expgui.exe
Ps ~ 50 Å