X-RAY DIFFRACTION

SOUMYAJIT SUR
October 2024

1 Introduction
X-ray diffraction (XRD) is a powerful analytical technique used to study the crystallographic structure,
phase identification, and material properties of a wide range of solid substances. In this experiment, we use
XRD to analyze the crystalline nature of silicon by measuring the diffraction of X-rays through the atomic
planes within the sample. The interaction between the incident X-rays and the crystal lattice produces a
diffraction pattern that reveals critical information about the material’s lattice parameters, crystallite size,
and any phase transitions.
The principle of XRD is based on Bragg’s Law, which relates the angle of incidence and diffraction to the
interplanar spacing in a crystal lattice. By interpreting the diffraction pattern, it is possible to determine
the structure and phase purity of a material, which is crucial for applications in materials science, chemistry,
and solid-state physics.
In this experiment, the sample material is exposed to monochromatic X-rays, and the resulting diffraction
peaks are recorded. These peaks correspond to specific crystallographic planes, and their positions and
intensities are analyzed to extract information about the material’s crystal structure, lattice parameters,
and possible impurities or defects.
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2 Aim:
• To calculate crystal structure of Si via calculating unit cell parameters (lattice parameters) from peak
positions of diffraction pattern, using Powder X-ray diffraction method.
• To underatand the Bragg”s Law and its relation to crystal structure.

3 Theory:
3.1 X-ray
• X-rays are high-energy electromagnetic radiation.They have energies ranging from about 200eV to
1MeV, which puts them between γ-rays and ultraviolet (UV) radiation in the electromagnetic spectrum.

3.2 X-ray Generation

3.2.1 Bremsstrahlung (Braking Radiation)
When high-speed electrons are decelerated or deflected by the nuclei of the target atoms, they lose energy,
which is emitted as X-rays. This radiation has a continuous spectrum because the energy loss can vary.

3.2.2 Characteristic X-rays

When an electron from the incident beam collides with an inner-shell electron of the target atom, it can
eject the inner-shell electron. The vacancy is then filled by an electron from a higher energy level, and the
energy difference between the levels is emitted as an X-ray. These X-rays have discrete energies that are
characteristic of the target material’s atomic structure.

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3.3 Steps in X-ray Production
3.3.1 Electron Generation
Electrons are typically generated by heating a filament (cathode) in an X-ray tube. The thermionic emission
process releases electrons from the heated filament.

3.3.2 Electron Acceleration

A high voltage is applied between the cathode and anode (target), accelerating the electrons towards the
anode. The potential difference determines the kinetic energy of the electrons, and hence the maximum
energy of the produced X-rays.

3.3.3 Electron Interaction with Target

When the accelerated electrons hit the target (usually made of tungsten or molybdenum), they interact
with the atoms in the target material. The interactions result in the production of Bremsstrahlung and
characteristic X-rays.

3.4 X-ray Diffraction

X-ray diffraction (XRD) is based on the principle that X-rays, when incident on a crystalline material,
can be scattered by the atoms in the crystal in a specific pattern. This phenomenon occurs because X-
rays have wavelengths on the same order of magnitude as the spacing between atomic planes in a crystal,
typically around 1–10 Å. The scattered X-rays from the crystal planes interfere with one another, leading to
constructive and destructive interference, which produces a diffraction pattern characteristic of the material’s
internal structure.
The foundational concept of XRD is governed by Bragg’s Law, which describes the condition for
constructive interference of the X-rays scattered by crystal planes. The law is given by:

nλ = 2d sin θ (1)
where:
• n is an integer (the order of diffraction),

• λ is the wavelength of the incident X-rays,

• d is the spacing between crystallographic planes in the material,
• θ is the angle between the incident X-rays and the crystal planes (the Bragg angle).
For constructive interference to occur, the path difference between X-rays scattered from successive planes
must be an integer multiple of the wavelength. This condition leads to sharp peaks at specific angles when
the scattered X-rays are in phase, producing a diffraction pattern that reflects the underlying structure of
the crystal.
Each material produces a unique diffraction pattern because the position and intensity of the diffraction
peaks depend on the arrangement of atoms in the crystal lattice. The peaks in an XRD pattern can be
indexed to specific crystallographic planes using known crystal structures and their corresponding lattice
parameters.

4 Experimental Details:
4.1 About the instrument
The direct photon counting HPAD allows for low-noise data collection and operation in 0D and 1D modes
for conventional XRD analysis and 2D mode for samples with coarse grain size and/or preferred orientation.
Additionally, a range of X-ray tube anodes, sample rotation and positioning accessories, and temperature
attachments are available to enhance the system’s versatility for qualitative and quantitative analyses.
The new MiniFlex X-ray diffractometer system is equipped with the SmartLab Studio-II, a comprehensive
powder diffraction analysis package, featuring advanced functionality like a fundamental parameter method
for accurate peak calculation, phase identification using the Crystallography Open Database (COD), and a
wizard for ab inito crystal structure analysis.

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4.2 Sample Preparation
Use the following procedure to correctly place the sample and insert it in the X-ray diffractometer.
• Pour the powder sample into the sample filling section of the glass sample holder.
• Flatten and compress the sample surface.
• Press the door lock button to unlock and open the door of the sample chamber on the front side.
• Mount the glass sample holder onto the standard sample stage.
• Close the sample chamber door and press the Door Lock button to lock the door.

5 Calculation:
5.1 Method to calculate miller indices
• Identification of peaks (peak positions).
• Determine sin2 θ.
• Calculate sin2 θ/sin2 θmin .
• Multiply by the appropriate integers.
• Select result from above that gives h2 + k 2 + l2 as an integer.
• Determine h,k and l values in accordance with the sequences of h2 + k 2 + l2 to identify the Bravis
lattice.
• λ for X-ray is 1.5406 Å

5.2 Observed Data

This is the observed data, when we do Powder XRD for Si.We get five peaks in diffraction pattren.

5.3 Observation Table

We calculate lattice parameters using

nλ = 2d ∗ sinθ

d = λ/(2sinθ)
Now we calculate lattice parameter using
p
a = d h2 + k 2 + l2

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 Figure 1: XRD pattern of Silicon

sin2 θ 2
Peak 2θ (degrees) sinθ sin2 θmin n. sinsin
2θ
θ
min
h2 + k 2 + l2 hkl a(Ã)
1 28.37 0.245 1 1·3 = 3 (n = 3) 12 + 1 2 + 1 2 (111) 5.455
2 47.24 0.401 2.678 8.034 ≈ 8 (n=3) 22 + 2 2 + 0 2 (220) 5.435
3 56.05 0.469 3.664 10.99 ≈ 11 (n=3) 32 + 1 2 + 1 2 (311) 5.445
4 69.08 0.567 5.356 16.068 ≈ 16 (n=3) 42 + 0 2 + 0 2 (400) 5.435
5 76.31 0.618 6.363 19.089 ≈ 19 (n=3) 32 + 3 2 + 1 2 (331) 5.435
6 87.95 0.694 8.03 24.09 ≈ 24 (n=3) 42 + 2 2 + 2 2 (211) 5.437

Table 1: Data collected for the determination of Lattice constant

6 Result:
• We get 5 planes for Si which are (1 1 1),(2 2 0),(3 1 1),(4 0 0), (3 3 1) and (221)
• The lattice parameter for Si is taking average of all parameters

aAvg = (5.455 + 5.435 + 5.445 + 5.435 + 5.435 + 5.437)/6

aAvg = 5.446Å.

• We know the lattice parameter for Si, which is 5.43102 Å.The error we get through this experiment is

error = 100 ∗ (5.446 − 5.431)/5.431

error = 0.2762%

• The crystal structure of Si is FCC, because we get (h k l) mixed (even and odd) miller indices i.e. the
crystal structure is FCC.

7 Precautions:
• X-rays can be hazardous to health, so it is crucial to minimize exposure.Always follow the ”As Low
As Reasonably Achievable”.

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• Ensure that all safety shields and covers are in place before operating the XRD instrument.These
shields are designed to contain X-rays and prevent exposure.
• Handle samples carefully to avoid contamination, which could affect the accuracy of the results.

• Ensure samples are mounted securely and correctly to avoid any movement or misalignment during
the measurement.
• Ensure that the XRD machine is properly grounded and that all electrical connections are secure and
in good condition to prevent electrical hazards.