X-Ray Diffraction

ME 217: X-ray Diffraction Experiment
OBJECTIVE
The purpose of this experiment is to introduce students to the use of X-ray diffraction techniques
for investigating various types of crystal structure encountered in metallic materials.
INTRODUCTION
X-rays were discovered in 1895 by the German physicist Wilhelm Conrad Rntgen. X-rays are highenergy electromagnetic radiation with energies ranging from about 200 eV to 1 MeV. X-ray
wavelengths vary from about 10 nm to 1 pm. (The shorter wavelength corresponds to the higher
energy of the radiation). The useful range of wavelengths for X-ray diffraction study is, however,
between 0.05 and 0.25 nm.
APPLICATION OF X-RAYS
X-ray diffraction (XRD) is a powerful technique to determine many structural and microstructural
parameters of crystalline materials including: (i) crystal structure of materials metals, alloys,
compounds, intermetallics, quasicrystals, semiconductors, and ceramic materials, (ii) solid-state
phase boundaries in phase diagrams, (iii) crystallite size and lattice strain in heavily cold-worked
materials, (iv) long-range order parameter in ordered alloys, (v) phase proportions in multi-phase
alloys and powder mixtures, (vi) textures, and (vii) magnitude of residual stresses.
PRODUCTION OF X-RAY
X-rays are produced when fast-moving free electrons are suddenly stopped by a metal target.
This is achieved in an X-ray tube consisting of two metal electrodes enclosed in a vacuum
chamber. Free electrons are produced by heating a tungsten filament cathode, maintained at a
high negative potential (usually about 30 to 50 kV). The free electrons produced are accelerated
toward the water cooled anode (which is normally at ground potential), collide and loss the energy
resulting X-ray generation. Less than 1% of the energy of the accelerated free electrons is
converted to X-rays, the rest is dissipated as heat.
Figure 01: Graphical presentation of X-ray emission: (a) an incident electron ejects a K shell
electron from an atom, (b) a hole is left in the K shell. (c) electron rearrangement occurs resulting
in the emission of an X-ray photon.
It is important to note that the X-ray beams are: (i) non visible, (ii) travel in all directions, and (iii)
penetrate encountering matter easily. X-rays are damaging because they penetrate the human
body and break up molecules of DNA in our cells. If these molecules do not repair themselves,
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they die. On the other hand, if the molecules are broken and they rejoin in a wrong way, then a
mutant cell is produced and this can lead to cancer. Precaution must be taken to avoid exposure to
X-ray.
X-RAY DIFFRACTION PHENOMENON
X-ray diffraction occurs when a wave encounters a series of regularly spaced obstacles: (i) have
spacings comparable in magnitude to the wavelength, and (ii) capable of scattering the wave.
Furthermore, diffraction is a consequence of specific phase relationships established between two
or more waves that have been scattered by the obstacles.
Figure 02: Demonstration of how two waves (labeled 1 and 2) that have the same wavelength
and remain in phase after a scattering event (waves 1 and 2) constructively interfere with one
another. The amplitudes of the scattered waves add together in the resultant wave.
Figure 03: Demonstration of how two waves (labeled 3 and 4) that have the same wavelength
and become out of phase after a scattering event (waves 3 and 4) destructively interfere with one
another. The amplitudes of the two scattered waves cancel one another.
A diffracted beam is defined as a beam consisting of a large number of scattered beams
reinforcing one another. The diffraction directions are governed by: (i) wavelength () of the
incident radiation, and (ii) nature of the crystalline sample.
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Figure 04: Schematic of an X-ray diffractometer.

BRAGG EQUATION (formulated by William Henry Bragg and William Lawrence Bragg, father and
son duo, in 1913) represents conditions for diffraction to occur from crystals by relating the
wavelength of the X-rays to the spacing of the atomic planes, d, in a crystal.
Figure 05: Schematic figure used to derive the Bragg equation. is the angle of incidence and d
is the interplanar spacing of the planes on which the X-ray beam is incident.
Braggs Equation
= 2 dhkl sin where dhkl =
a
h + k 2+ l 2
2
Braggs Law specifies that diffraction occur from atoms positioned only at cell corners. Atoms
situated at other sites (e.g., face and interior unit cell positions as with FCC and BCC) act as extra
scattering centers and produce out-of-phase scattering at certain Bragg angles. For example: To
analyze X-ray diffraction data, the crystal planes which diffract must be known for each type of
crystal structure. For the BCC structure, diffraction occurs only on planes whose Miller indices when
added together (h + k + l) total to an even number (see Table 1). In the case of the FCC crystal
structure, the principal diffracting planes are those whose Miller indices are either all even or all
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odd (zero is considered even); planes with mixed odd and even indices give rise to zero intensity
and their diffraction peaks do not appear in the pattern.
Table 1 - Diffraction Planes in Cubic Crystals.
Bravais Lattice
BCC
FCC
Constructive Interference
(Reflections Present)
(h + k + l) = Even
(h,k,l) All Odd or All Even
Destructive Interference
(Reflections Absent)
(h + k + l) = Odd
(h,k,l) Not All Odd or All Even
CRYSTAL STRUCTURE DETERMINATION

Full structure determination consists of three steps:
(a) calculation of the size and shape of the unit cell from the angular positions of the diffraction
peaks, i.e., determination of the six lattice parameters of the unit cell. But, before we could
do this, we need to identify the planes from which diffraction is occurring and this step is
known as indexing of the XRD pattern.
(b) computation of the number of atoms per unit cell from the volume of the unit cell, chemical
composition, and its measured density, and
(c) determination of the atom positions within the unit cell from the relative intensities of the
diffraction peaks.
We will consider only step (a), i.e., index the XRD pattern and determine the shape (Bravais
lattice) and size (lattice parameters) of the unit cell.
ASSIGNMENT
Aluminum sample
The diffraction patter shows the results of an x-ray diffraction experiment in the form of intensity of
the diffracted peak values versus 2 diffraction angle for an aluminum sample. If x-rays with a
wavelength of 0.1542 nm were used, determine:
a)
b)
c)
d)
e)
the indices of the planes that produced each of the peaks,

the interplanar distances between the planes producing the first, second, and third peaks,
the lattice parameter,
the atomic radius for aluminum, and
compare with the standard atomic size for aluminum
Figure 06 A typical X-ray diffraction pattern of aluminum metal powder recorded using Cu K
radiation.
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Unknown Metal Sample

The diffraction patter shows the results of an x-ray diffraction experiment in the form of intensity of
the diffracted peak values versus 2 diffraction angle for an unknown metal. If x-rays with a
wavelength of 0.1542 nm were used, determine:
a)
b)
c)
d)
e)
the
the
the
the
the
crystal structure of the metal

indices of the planes that produce each of the peaks
interplanar distances between the planes producing the first, second, and third peaks.
lattice parameter of the metal
most probable metal that produced this diffraction pattern
Figure 07 A typical X-ray diffraction pattern of unknown metal powder recorded using Cu K
radiation.
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Figure 08 Possible diffracted planes for different cubic unit cells
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ME 217: X-ray Diffraction Experiment

Figure 04: Schematic of an X-ray diffractometer.

= 2 dhkl sin where dhkl =

CRYSTAL STRUCTURE DETERMINATION

the indices of the planes that produced each of the peaks,

Unknown Metal Sample

crystal structure of the metal

Figure 08 Possible diffracted planes for different cubic unit cells

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