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Abstract: Diffraction occurs when electromagnetic radiation is scattered off of a regular periodic
system of objects (atoms, in our case) and the distance between the centers of these objects is
approximately the same as the wavelength of the radiation. X-Rays are useful in identifying
crystal structures since x-ray radiation represents the spectrum of radiation around 0.1
nanometers, which is an acceptable approximation of the size of atoms and ions. X-ray diffraction
provides angle values for the maximum intensity of scattering (in 2 ), which in turn can be used
to calculate the distance between lattice planes. These distances are then used in conjunction with
the Miller indices to calculate the lattice parameters for that particular compound.
Raina N. Smith
PHY450
February 2, 1998
Introduction
After Wilhelm Roentgen discovered x-rays in 1895, many people worked diligently to determine
their characteristics. It was the determination that x-rays were a form of electromagnetic
radiation, but with wavelengths much shorter than visible light, that caused Max von Laue to
propose that crystal lattices could be used as three-dimensional gratings.1 He said that the waves
scattered through such a grating should be the right wavelength to produce observable
interference. Von Laue designed the experiment which was consequentially performed by Walter
Friedrich and Paul Knipping. The results convincingly showed both the wave-nature of x-rays,
and the proposed lattice structure of crystals. William Lawrence Bragg then determined the
equation known as Bragg's law:
nλ = 2d sin θ
where n = 1, 2 ,3 , ... and d is the distance between lattice planes, as well as developing an
apparatus with William Henry Bragg (his father) known as a Bragg Spectrometer which rotated
the crystal and detector around a fixed x-ray beam to determine the intensity of the diffracted
beam as a function of the scattering angle. It is this same principle which is used in modern x-ray
diffraction techniques.
My experiment consists of using an x-ray diffractometer and Bragg's law to determine the
distance between lattice planes corresponding to the angle of each peak of intensity for several
samples, and to then determine the Miller indices of the crystal plane responsible for each
intensity. I will then calculate the lattice parameters (length of unit cell edges) to determine the
crystal structure of the samples.
Experimental Method
The apparatus used will be the Rigaku Geigerflex X-Ray Diffractometer as shown below in
Figure 1. It consists of an x-ray tube to which is applied a high voltage, a goniometer which
measures the angle between the x-ray beam incident to the sample and the diffracted beam (see
Figure 2), and a scintillation-type counter. Electric signals sent by the counter are counted to get
a rate-per-second, which is then converted to the corresponding voltages by the ratemeter, and
recorded on the chart recorder.2
2
Raina N. Smith
PHY450
February 2, 1998
Scintillation
X-Ray Tube Counter
Bragg angle
diffraction angle
Sample
3
Raina N. Smith
PHY450
February 2, 1998
The taking of data will begin, and will be recorded on chart paper as intensity versus 2 . These 2
values are used to calculate the value for d in Bragg's law, which can then be looked up in
reference tables to obtain the Miller indices associated with that peak. The lattice parameter a is
the unit cell edge width of the crystal. It is related to the distance d and the Miller indices hkl as
follows (for a cubic system)4:
a = d hkl h 2 + k 2 + l 2
I have listed the calculated interplanar distances and peak intensities, and the proposed Miller
indices based on them. The peak intensities were calculated based on a peak-height/max. peak-
height ratio which was then normalized to 100. The distance between lattice planes was
calculated using Bragg's law with n=1.
4
Raina N. Smith
PHY450
February 2, 1998
5
Raina N. Smith
PHY450
February 2, 1998
6
Raina N. Smith
PHY450
February 2, 1998
Accepted values for the data are as follows (please note that the Al sample was a foil, and not a
power—solid Al information was not available):
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Raina N. Smith
PHY450
February 2, 1998
Choosing the two acceptable samples, KCl sample number 4 and the KBr sample, calculated
values for the lattice parameters are as follows:
As would be expected in cubic crystals, the calculated lattice parameters are approximately equal
for each of the samples irregardless of which plane (Miller Indices) caused the diffraction peak.
Conclusion
While most of the data taken contained extraneous peaks and switched intensities of peaks, two
of the samples (KCl sample number 4 and the KBr sample) produced data which resulted in
acceptable calculations of the lattice parameters for each, substantiating that both samples were
indeed cubic crystalline forms.
I believe that having the correct chart paper on hand would have helped tremendously in obtaining
more accurate results, as would having a mortar and pestle to assure uniformly pulvarized
samples. These steps should be taken before any more powder data is taken (as well as repairing
the leak in the system).
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Raina N. Smith
PHY450
February 2, 1998
9
1
Thornton, Stephen T. and Andrew Rex, Modern Physics for Scientists and Engineers (Saunders College Publishing, Fort
Worth, TX, 1993), p. 176.
2
Rigaku Corporation, General Operating Procedure for Rigaku Geigerflex X-Ray Diffractometer System, Models #
CN2028 and #CN2038, Manual # ME200DM. pp. 3-4.
3
Rigaku Corporation, General Operating Procedure for Rigaku Geigerflex X-Ray Diffractometer System, Models #
CN2028 and #CN2038, Manual # ME200DM. pp. 5-7.
4
Shackelford, James F., Introduction to Materials Science for Engineers, Second Edition (MacMillan Publishing
Company, New York, 1988), p.110.
5
JCPDS—International Centre for Diffraction Data, Powder Diffraction File, Alphabetical Index, Inorganic Phases 1981.