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2 Introduction To XRPD Data Analysis
2 Introduction To XRPD Data Analysis
2 Introduction To XRPD Data Analysis
De
Intensity (Counts)
sample
to
t ec
5000
40
45
10000
35
50
55
Cristobalite
Glass
15
20
25
30
35
40
The X-ray diffraction pattern is a fingerprint that lets you figure out what
is in
your sample.
Scott A Speakman, Ph.D.
Slide # of 20
speakman@mit.edu
Quartz
Cristobalite
Glass
15
20
25
30
35
Position [2Theta] (Cu K-alpha)
40
15
20
25
30
35
Slide # of 20
40
Slide # of 20
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Slide # of 20
Kalpha1
Kalpha2
Kalpha1
Kalpha2
The k-alpha1 and k-alpha2 peak doublets are further apart at higher angles 2theta
The k-alpha1 peaks always as twice the intensity of the k-alpha2
At low angles 2theta, you might not observe a distinct second peak
Slide # of 20
This is an example of a bad match between the data and the reference
patternScott A Speakman, Ph.D.
Slide # of 20
speakman@mit.edu
Hematite, syn;
Rutile, syn;
Hematite, syn;
Rutile, syn;
400
Anatase, syn;
Anatase, syn;
Rutile,
syn;
Hematite,
syn;
Anatase, syn;
Hematite, syn;
Rutile, syn;
Hematite, syn;
Rutile, syn;
1600
Hematite, syn;
3600
Anatase, syn;
0
25
30
35
Position [2Theta] (Copper (Cu))
40
45
The pattern shown above contains equal amounts of TiO2 and Al2O3
The TiO2 pattern is more intense because TiO2 diffracts X-rays more efficiently
With proper calibration, you can calculate the amount of each phase
present in the sample
Scott A Speakman, Ph.D.
Slide # of 20
speakman@mit.edu
However, different instrument configurations can change the peak width, too
Slide # of 20
speakman@mit.edu
Slide # of 20
24.179 deg
d= 3.6779
1000
25.321 deg
d= 3.5145
500
0
23
24
25
Position [2Theta] (Copper (Cu))
26
Slide # of 20
nts
Width=0.007 rad
XS ~ 19 nm
Width=0.002 rad
XS> 90 nm
1000
Size
500
0
23
24
25
Position [2Theta] (Copper (Cu))
26
Non-uniform lattice strain and defects will also cause peak broadening
Careful evaluation is required to separate all of the different potential causes of peak broadening
Slide # of 20
Counts
3600
1600
400
0
25
30
35
Position [2Theta] (Copper (Cu))
40
45
If you use many peaks over a long angular range (for example, 7+ peaks over a 60
2theta range), you can:
Calculate and correct for specimen displacement when solving lattice parameters
Calculate and account for microstrain broadening when calculating crystallite size
Improve precision by one or two orders of magnitude
Slide # of 20
Peak search
Analysis of the second derivative of diffraction data is used to identify
likely diffraction peaks
Peak information is extracted by fitting a parabola around a minimum in
the second derivative
This method is fast but the peak information lacks precision
Profile fitting
Slide # of 20
Intensity (a.u.)
28.5
29.0
2(deg.)
Slide # of 20
29.5
30.0
Peak areas are much more reliable than peak heights as a measure of
intensity.
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