Mechanical Engineering Department

MEEN 225 Engineering Materials Laboratory

Experiment # 5

X-ray Diffraction (XRD)

Group Members:
Saif Alremeithi 100050053
Khalifa Alshehhi 100045464
Ahmad Alzain 100053848
Taleb Ameeri 100049719

Experiment Performed on: 27/04/2021

Lab Instructor/s: Ayesha Alkhoori ; Amani Alhammadi

The following experiment analyzes two salt samples; Hymnal salt and table salt; through X-
ray diffraction analysis (XRD) to determine the degree of crystallinity, crystallite size, and the
inter-planar spacing. The Bruker XRD machine will be used to perform the analysis. After setting
up the samples in the machine and running the test, the data is plotted to form the diffraction
pattern graphs that indicate the peaks at certain angle θ which then is used to calculate the
crystallite size and the spacing. The results showed similar number and places of the peaks
compared to the ICDD indicating the purity of the two samples with the Hymnal salt showing a
higher intensity at the peaks.

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Table of Contents
Abstract..................................................................................................................................2
1. Introduction...................................................................................................................4
2. Experimental Setup........................................................................................................4
3. Results...........................................................................................................................4
4. Analysis/Discussion.......................................................................................................4
5. Conclusions....................................................................................................................4
References..............................................................................................................................6

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 1. Introduction

X-Ray Diffraction Analysis (XRD) is a common method used in labs to determine the
crystallographic structure of a certain material. Furthermore, it functions by radiating X-Rays
waves upon crystal atoms and scatters them accordingly. The normal arrays result in a normal
spherical array and both consecutive, constructive waves as determined by Bragg’s Law:
2dsinθ = nλ, here d is the spacing between diffracting planes, θ is the incident angle, n is an
integer, and λ is the beam wavelength. The benefit of said XDR is to find out the material’s
phases, and orientation. The objective of this lab is to study the degree of crystallinity, crystal
structure, crystallite size of the material, then compare it to the standard ICDD (International
Centre for Diffraction Data).

2. Experimental Setup

Figure 2
Figure 1 Figure 3

Figure 1 shows the Bruker XRD machine that will be used in the experiment.

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The experiment starts with loading the samples (figure 3) into the holders shown in figure 2, the
sample should be placed in the center of the holder. Using another holder, level the surface of
the sample to have a smooth surface to ensure accurate results. After opening the XRD
machine, place the holder with the sample into the sample load then close the machine and run
the XRD software. When the software loads up, turn on the X-ray. The next step is to set up the
parameters, adjust the starting angle around 4⁰ with an angle no smaller than to protect the
detector from overexposure. As for the stop angle set it to 120⁰ and set up the increment based
on the resolution needed making sure not to make it too low and cause unnecessary noise.
After setting up the parameters start the experiment and wait for the machine to end the
experiment then save the data in the format required.

After finishing the experiment, make sure to close the software and clean the sample holders
with water for plastic holders and alcohol rub for metal holders.

3. Results
Hymnal Salt Diffraction Pattern
16000
14000
12000
10000
Intensity

8000
6000
4000
2000
0
10 20 30 40 50 60 70 80 90
2θ

Diffraction pattern of sample 1

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 Table Salt Diffraction Pattern
8000

7000

6000

5000

4000

3000

2000

1000

0
10 20 30 40 50 60 70 80 90

Diffraction pattern of sample 2

4. Analysis/Discussion

- The results of sample 1 and sample 2 show that the samples have a high degree of
crystallinity as the peaks appear to be sharp intense peaks rather than wider peaks that
indicate amorphous structures. However, the peak of sample 1 (Hymnal salt) has a
higher intensity peak indicating bigger crystal structures than sample 2 (table salt)
despite being made from the same material (NaCl)

- Moreover, the results can be directly compared to the standard ICDD showing that both
samples are relatively pure having the same positions and numbers of peaks as in the
standard data. Comparatively, both samples peak at higher intensities than the standard
data and this can be explained since the standard data used powdered NaCl while the
samples used crystals.

Sample 2θ θ (rad) Intensity β (rad) Crystallite size, D Spacing, d

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 K ∙λ 0.89 ( 0.15418 ×10−9 )
D= = =42.74 nm
β ∙ cos θ 0.0033388 × cos ( 0.27804 )

n∙ λ 1 × ( 0.15418 × 10−9 )
d= = =0.2809 nm
2 ∙ sinθ 2 ×sin 0.27804

5. Conclusions

As shown from the above study, Hymnal salt showed a higher intensity in
comparison to table salt, which essentially indicates bigger crystals used in the sample.
Moreover, the number of peaks along with the θ the peaks are associated with are
similar indicating that both samples are made up of the same materials. In other words,
the intensity of the peaks indicated the size of the crystals while the angle it forms a
peak on relates to the material itself. The two samples showed equivalent graphs to the
ICDD graph of NaCl with higher intensity since ICDD samples are in powdered form.

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References