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by Two-dimensional
XRD
Bob He
Bruker AXS, Inc.
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Two-dimensional XRD
Particle Size Analysis – conventional methods
Particle Size Analysis –XRD2 method
⎡ h x ⎤ ⎡ − sin θ ⎤
⎢ ⎥ ⎢ ⎥
h L = ⎢ h y ⎥ = ⎢ − cos θ sin γ ⎥ Diffraction rings (blue) in
⎢ ⎥ ⎢ ⎥ the laboratory axes (red).
⎢⎣ h z ⎥⎦ ⎢⎣ − cos θ cos γ ⎥⎦
1 nm 10 nm 100 nm 1 µm 10 µm 100 µ m 1 mm
Scherrer equation: Cλ
t=
B cos θ
where λ is wavelength (Å), B is FWHM (radians) corrected
for instrument broadening, θ is Bragg angle, C is a crystal
shape factor from 0.9~1.
For Gaussian profiles, 2 2 2
B =U − S
while for Cauchy profiles,
B =U − S
where B is the corrected FWHM for crystallite size
calculation by Scherrer equation, and U and S are the
FWHM’s of the unknown and standard peaks, respectively.
Left: NIST SRM 660, LaB6. Profile fitting of the peak shown gives a FWHM
of 0.162º with a Gaussian profile and 0.133º with a Cauchy.
Right: Cu (111) peak from a semiconductor tab tape. Profile fitting with a
Cauchy function for a peak at 43.455º 2θ gives a FWHM of 0.300º.
Using LaB6 as an instrumental broadening standard with a Cauchy FWHM
of 0.133º, the corrected FWHM is 0.167º, and the Scherrer equation gives
a crystallite size of 512 Å.
13 Bruker Confidential 05.05.2009
XRD2: Particle size measurement by γ profile analysis:
XRD Pattern
Debye Cone
Incident Beam
Sample
s-so
Ω
so
s
β2
β β1
β ∆γ
140
To cancel out the effects of
90
the overall intensity
fluctuation (texture, etc.), a
2nd order polynomial trend line
40
threshold line.
80
70
(111)
60
50
Every two intersections of γ-
40 profile with the threshold line
represents a crystallite.
30
20
10
0
γ
-109 -104 -99 -94 -89 -84 -79 -74
Calibration Results:
(hkl) Phkl 2θ ∆ω Ns k
(100) 6 21.36 38 23 0.1217
(110) 12 30.38 46 41 0.1106
(111) 8 37.44 42 38 0.1281
The average scaling factor k is 0.12 in this calibration. The system can
then be used to measure the crystallite size of unknown materials if the
data can be collected in approximately the same condition.
It is always necessary to calibrate the system with a known standard,
preferably with a comparable sample geometry and crystallite size.
For reflection mode, it is critical to have a standard with a comparable
linear absorption coefficient so as to have similar penetration.
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