X-Ray Diffraction and Lattice

Parameter Determination

J. Ernesto Indacochea
University of Illinois at Chicago
Materials Engineering
CME 470 J. Ernesto Indacochea UIC
 X-Ray Diffraction
Determination of Crystal Structures
Nature of X-Rays:
q
X-rays are electromagnetic
waves with wavelengths ~ 0.05 K
- 0.25 nm (0.5 -2.5).
Wavelength of visible light is
~ 600 nm (6000).
c
E h h

K
c
h
E x ray x ray vl
;
Evl h
c x ray
vl
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CME 470 J. Ernesto Indacochea UIC
 X-Ray Diffraction
Determination of Crystal Structures
Production of X-Rays:
A voltage of 35,000 volts is applied between the
cathode and anode target metal in the x-ray
tube.
Then the electrons released from the W-filament
strike the metal target (anode), x-rays are
produced.
Note: 98% of the energy is converted into heat.

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CME 470 J. Ernesto Indacochea UIC
 X-Ray Diffraction
Determination of Crystal Structures
Diffraction Phenomena:
Occurs as the wave encounters a
series of regularly spaced
obstacles which scatter the wave.
These scattering centers (atoms),
have spacing comparable in
magnitude to the wavelength.
Diffraction results from specific
phase relationships established
between the waves scattered by
the scattering atoms (centers).

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CME 470 J. Ernesto Indacochea UIC
 X-Ray Diffraction

f , d hkl 2 d hkl sin

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CME 470 J. Ernesto Indacochea UIC
 X-Ray Diffraction
Determination of Crystal Structures

Al-powder

X-Ray spectrum for aluminum powder.

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CME 470 J. Ernesto Indacochea UIC
 Interplanar Spacing in
Cubic Structures
ao
d cubic

hkl
h 2
k2 l2

Interplanar spacing of Al (110) planes:

aoAl
d Al

110
1 2
12 0 2
aoAl
d Al
110
2

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CME 470 J. Ernesto Indacochea UIC
 Diffraction Angle or Direction
Using Braggs law in combination with d-
spacing:
a
2 d hkl sin cubic o
d
h k l hkl 2 2 2

ao
2 sin
h 2
k2 l2

sin h 2
k2 l2
2
ao 2 ao
h 2
k2 l2
2

2
sin
2

2
h k 2
l 2

4 a o
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CME 470 J. Ernesto Indacochea UIC
 Intensity of Diffracted Beam
The particular arrangement of the atoms in the
crystal lattice will determine if diffraction occurs =>
only certain planes will diffract.
Because of this factor, x-rays determines the
crystal structure of a material.
Note also that the peak intensities of the diffracted
beams are not the same

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CME 470 J. Ernesto Indacochea UIC
 X-Ray Diffraction
X-Ray spectrum of Fe
Cu-Kradiation: = 0.1542 nm

Al-powder
X-Ray spectrum of Al

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CME 470 J. Ernesto Indacochea UIC
 Intensity of Diffracted Beam
Each atom has an atomic scattering factor, f,
defined by:
amplitude of wave scattered by atom
f
amplitude of wave scattered by one electron

f is a measure of the scattering efficiency of all

electrons in the atom.

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CME 470 J. Ernesto Indacochea UIC
 Intensity of Diffracted Beam
X-Ray also interacts with the electrons in an atom
through scattering, which may be understood as the
redistribution of the of the X-Ray energy spatially.
f is a measure of the scattering efficiency of all
electrons in the atom.

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CME 470 J. Ernesto Indacochea UIC
 Intensity of Diffracted Beam
f is equal to Z (atomic number) if
scattering is in the same direction as
the X-ray => all scattered waves are in
phase.
Therefore, f is a function of the
scattering direction.
All atoms are packed close to each
other in a crystal:
The resultant scattered wave from one atom affects those
emitted from nearby atoms.
Hence, the resultant wave from all atoms is the sum of all the
scattered waves coming from all the atoms.

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CME 470 J. Ernesto Indacochea UIC
 Intensity of Diffracted Beam

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CME 470 J. Ernesto Indacochea UIC
 Intensity of Diffracted Beam

F is called the structure factor.

The intensity of the diffracted beam F2

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CME 470 J. Ernesto Indacochea UIC
Structure Factors for Cubic Structures

F is independent of h, k, and l and is the same for all

diffracted beams.
All planes will have a diffracted beam (wave)
All (hkl) diffracted lines will appear

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CME 470 J. Ernesto Indacochea UIC
Structure Factors for Cubic Structures

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CME 470 J. Ernesto Indacochea UIC
Structure Factors for Cubic Structures
Face Centered Cubic:
# of atoms per unit cell: 4
Coordinates of the atom:
(u1 v1 w1), (u2 v2 w2), (u3 v3 w3), (u4 v4 w4)
(0,0,0), (, , 0), (, 0, ), (0, , )
= [1 + (+) + (+) + (+) ]

Case 1: h, k, l are either all odd or all even (unmixed)

F = 4f => F2 = 16 f
Case 2: h, k, l are mixed
F=0 => F2 = 0
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CME 470 J. Ernesto Indacochea UIC
Structure Factors for Cubic Structures

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CME 470 J. Ernesto Indacochea UIC
 X-Ray Diffraction Techniques

CuO nanostructure x-ray pattern

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CME 470 J. Ernesto Indacochea UIC
 X-Ray Diffraction
Determination of Crystal Structures
Problem: Determine the d-spacing for the (111) plane, the
lattice parameter ao, and the atomic radius r for Al. (Refer to
the X-Ray spectrum for Al).
2 38o 19o for (111)
0.1542 nm
2 d hkl sin d 111 0.237 nm
2 sin 2 sin 19 o

ao
d hkl ao d hkl h 2 k 2 l 2 d (111) 12 12 12
h2 k 2 l 2
ao 0.237 3 nm 0.237 3 nm 0.410nm
4r a 2
ao r o 0.144 nm
2 4

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CME 470 J. Ernesto Indacochea UIC