XRD - Materials Science Refresher Course

Identification of Crystal Structure by X-ray
Diffraction (XRD) Technique

Indexing a diffraction pattern from cubic
materials
Calculations of Lattice Parameters X-ray
Diffraction (XRD) Technique
Fourth Year BSc, Phys 4107: Condensed Matter Physics

Second Year BSc Honours, Phys 4207: Condensed Matter Physics
MSc Qualifying, Phys 5207: Condensed Matter Physics
Dr Aye Aye Thant

Dr Nwe Ni Hlaing
Dr Than Htike Win
U Aye Min Oo
Department of Physics, University of Yangon

 Identification of Crystal Structure by X-ray Diffraction (XRD)
Technique
Aim : To study X-ray Diffraction (XRD) technique and its application to identify the
crystal structure
Objectives :
- Know the concept of Powder X-ray diffraction
- Understand the concept of diffraction in crystals
- Derive Bragg’s law and understand its significance
- Identify the crystal structure
Bragg’s Law of Diffraction
When a collimated beam of X-rays strikes pair of parallel lattice planes in a crystal,
each atom acts as a scattering center and emits a secondary wave. All of the secondary
waves interfere with each other to produce the diffracted beam.
Bragg provided a simple, intuitive approach to diffraction:
- Regard crystal as parallel planes of atoms separated by distance d
- Assume specular reflection of X-rays from any given plane
Peaks in the intensity of scattered radiation will occur when rays from successive planes
interfere constructively.
Figure 1 Bragg’s Law (condition for diffraction)

Derivation of Bragg’s Law
- Lower ray travels farther by the distance: xy+yz

- When the emerging rays are in phase and to give constructive interference: λ
= xy+yz
- It can be shown that xy = d sinθ and yz = d sinθ
λ = 2d sinθ
where, λ = the wavelength of the incident X-ray beam,
d = the interplanar spacing in a crystal, and
2θ = the angle between the diffracted beams and transmitted beams.
No peak is observed unless the condition for constructive interference (δ = n λ, with n,
an integer) is precisely met. When Bragg’s Law is satisfied, “reflected” beams are in
phase and interfere constructively. Specular “reflections” can occur only at these angles.
Identification of the Crystal Structure
X-Ray Diffraction (XRD) is a non-destructive technique for analyzing a wide range of
materials, including fluids. Its applications include qualitative and quantitative phase
analysis, crystallography, structure and relaxation determination, texture and residual
stress investigations, controlled sample environment, micro-diffraction and nano-
materials.
The diffraction beam from a crystal is built up of rays scattered by all the atoms of the
crystal which lie in the path of the incident beam.
𝜆 = 2𝑑 𝑠𝑖𝑛𝜃 (1)
The phenomenon of scattering of incident x-rays by crystal atoms (atomic planes),
producing a diffraction pattern that yields information about the structure of the crystal.
The angular positions of diffracted peaks give information on the properties of size and
type of the unit cell while the intensities of diffracted peaks gives information on the
types of atoms in the unit cell.
Figure 2 Scattering of incident x-rays by crystal atoms (atomic planes) with Interplanar
spacing (d), producing a diffraction pattern
Figure 3 X-ray Diffraction configuration
Figure 4 X-ray diffractometer with components (X-ray Source, Flat specimen, Filters,
Slit, Monochromator, Detector
Exercise
The crystal structure of SrTiO3 is cubic with a unit cell edge a = 3.90 Å. Calculate the
expected 2θ positions of the peaks (100), (110), (111) in the diffraction pattern, if the
radiation is Cu Kα (λ=1.54Å).
Step 1 Calculate the interplanar spacing, d, for each peak
Step 2 Use Bragg’s law to determine the 2θ value
Step 3 Identify structure of the XRD pattern below based on you results obtained.
Figure 5 Powder Diffraction Pattern characterized by Powder X-ray Diffractometer
Extra Self-study: Why are the intensities of the peak different for different planes?
 Indexing a diffraction pattern from cubic materials
 Primitive h2+ k2+ l2 = 1,2,3,4,5,6,8,9,10,11,12,13,14,16…

 Body-centered h + k + l = 2,4,6,8,10,12,14,16…
2 2 2
 Face-centered h2+ k2+l2 = 3,4,8,11,12,16,19,20,24,27,32…
Ref: Crystal Structure Determination I

Dr. Falak Sher Pakistan Institute of Engineering and Applied Sciences
Ref: X-Ray Diffraction Crystallography: Introduction, Examples and Solved
Problems
Yoshio Waseda, Eiichiro Matsubara, Kozo Shinoda
 Calculations of Lattice Parameters
Aim : To study X-ray Diffraction (XRD) technique and its application to identify the
crystal structure and calculate the lattice parameters
Objectives :
- Know the concept of Powder X-ray diffraction
- Understand the concept of diffraction in crystals
- Derive Bragg’s law and understand its significance
- Identify the crystal structure and calculate the lattice parameters
Bragg’s Law of Diffraction
When a collimated beam of X-rays strikes pair of parallel lattice planes in a crystal,
each atom acts as a scattering center and emits a secondary wave. All of the secondary
waves interfere with each other to produce the diffracted beam.
Bragg provided a simple, intuitive approach to diffraction:
- Regard crystal as parallel planes of atoms separated by distance d
- Assume specular reflection of X-rays from any given plane
Peaks in the intensity of scattered radiation will occur when rays from successive planes
interfere constructively.
Figure 1 Bragg’s Law (condition for diffraction)

Derivation of Bragg’s Law
- Lower ray travels farther by the distance: xy+yz
- When the emerging rays are in phase and to give constructive interference: λ
= xy+yz
- It can be shown that xy = d sinθ and yz = d sinθ
λ = 2d sinθ
where, λ = the wavelength of the incident X-ray beam,
d = the interplanar spacing in a crystal, and
2θ = the angle between the diffracted beams and transmitted beams.
No peak is observed unless the condition for constructive interference (δ = nλ, with n,
an integer) is precisely met. When Bragg’s Law is satisfied, “reflected” beams are in
phase and interfere constructively. Specular “reflections” can occur only at these angles.
Identification of the Crystal Structure
X-Ray Diffraction (XRD) is a non-destructive technique for analyzing a wide range of
materials, including fluids. Its applications include qualitative and quantitative phase
analysis, crystallography, structure and relaxation determination, texture and residual
stress investigations, controlled sample environment, micro-diffraction and nano-
materials.
The diffraction beam from a crystal is built up of rays scattered by all the atoms of the
crystal which lie in the path of the incident beam.
𝜆 = 2𝑑 𝑠𝑖𝑛𝜃 (1)
The phenomenon of scattering of incident x-rays by crystal atoms (atomic planes),
producing a diffraction pattern that yields information about the structure of the crystal.
The angular positions of diffracted peaks give information on the properties of size and
type of the unit cell while the intensities of diffracted peaks gives information on the
types of atoms in the unit cell.
Figure 2 Scattering of incident x-rays by crystal atoms (atomic planes) with Interplanar
spacing (d), producing a diffraction pattern
Figure 3 X-ray Diffraction configurations
Figure 4 X-ray diffractometer with components (X-ray Source, Flat specimen, Filters,
Slit, Monochromator, Detector
Calculation of Lattice Parameters
The lattice spacing for the crystal structures are related to the Miller indices as shown
in Equation 2 to Equation 5.
For Cubic: a=b=c
(2)
For Orthorhombic: a≠b≠c
(3)
For Tetragonal: a=b≠c
(4)
For Hexagonal: a=b≠c, α=β=90˚; γ =

120˚
(5)
For cubic structure, combining the relation (Equation 2) with Bragg's law (Equation 1),
then we get Equation 7 to calculate lattice parameters.
4ao2
  4d sin   2
2 2 2
sin 2 
 
(6)
h k l
2 2
2 2 2
4ao2
 h  k 2
 l 2
 
4ao2
s  sin 2
 (7)
Exercise 1
The crystal structure of SrTiO3 is cubic with a unit cell edge a = 3.90 Å. Calculate the
expected 2θ positions of the peaks (100), (110), (111) in the diffraction pattern, if the
radiation is Cu Kα (λ=1.54Å).
Step 1 Calculate the interplanar spacing, d, for each peak
Step 2 Use Bragg’s law to determine the 2θ value
Step 3 Identify structure of the XRD pattern below based on you results obtained.
Figure 5 Powder Diffraction Pattern characterized by Powder X-ray Diffractometer
Extra Self-study
Why are the intensities of the peak different for different planes?
Exercise 2
Calculate the lattice parameter of MgFe2O4 which is a cubic spinel structure by using
Equation 7. The radiation is Cu Kα (λ=1.54Å) and its XRD pattern and data are
presented in Figure 6 and Table 1 respectively.
140
(311)
120
100
80 (440)
counts
60
(511)
40 (220)
(400)
20 (422) (533)
(620)
0
-20
20 30 40 50 60 70 80
2θ (deg.)
Figure 6 Powder Diffraction Pattern of MgFe2O4
Table 1 the (hkl) plane, 2θ value and intensity for XRD pattern of MgFe2O4
2θ (deg.) (hkl) plane Intensity

30.1921 220 35.848
35.4968 311 98.491
43.1972 400 26.783
53.5328 422 15.451
57.0579 511 43.292
62.6364 440 67.146
71.0897 620 7.0557
74.1014 533 14.611
Extra Self-study
What information can we get from Powder XRD; peak positions, peak intensities and
peak shapes and widths?

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Identification of Crystal Structure by X-ray

Diffraction (XRD) Technique

Fourth Year BSc, Phys 4107: Condensed Matter Physics

Dr Aye Aye Thant

Department of Physics, University of Yangon

Figure 1 Bragg’s Law (condition for diffraction)

- Lower ray travels farther by the distance: xy+yz

Figure 5 Powder Diffraction Pattern characterized by Powder X-ray Diffractometer

 Primitive h2+ k2+ l2 = 1,2,3,4,5,6,8,9,10,11,12,13,14,16…

 Face-centered h2+ k2+l2 = 3,4,8,11,12,16,19,20,24,27,32…

Ref: Crystal Structure Determination I

 Calculations of Lattice Parameters

Figure 1 Bragg’s Law (condition for diffraction)

For Cubic: a=b=c

For Orthorhombic: a≠b≠c

For Tetragonal: a=b≠c

For Hexagonal: a=b≠c, α=β=90˚; γ =

Figure 5 Powder Diffraction Pattern characterized by Powder X-ray Diffractometer

2θ (deg.) (hkl) plane Intensity

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