MSE 503

Material Characterization
Laboratory Report

X-Ray Diffraction

By:
IQBAL AZKA AL HAMID
g202390350

Material Science and Engineering Department

College of Chemicals and Materials

KING FAHD UNIVERSITY OF PETROLEUM AND MINERAL

DHAHRAN, SAUDI ARABIA
ABSTRACT
This report is a summary and calculation of the experimental X-ray diffraction technique that was

done in the Research Institute of KFUPM at Laboratory 3201. The purpose of this activity is to

define and analyze the unknown material (sample named MSE 503-03). The analyzed data output

was the investigated material’s data such as the type of the material whether it is crystalline or

amorphous, also the lattice parameter, the crystal structure, the grain size, and the strain of the

material unknown sample. This experiment uses the XRD instrument named Rigaku Mini Flex II.

The analysis started by diffracting the material sample with an X-ray in a certain condition and

parameter. The graph will be shown as the result of the diffracting process, that graph continues to

be analyzed with 3 software which are Standard Measurement Software, PDF-2 Release 2022, and

PDXL2. The analysis includes the recognition of the crystalline composition of the material, the

structure of the material, and the lattice parameters. All of that result data compared with the

database specifically uses the PDF-2 Release 2022 software to match the result’s graph and the

database’s graph. The data of the peak number also continues to be analyzed by scherrer equation to

define the grain size and the strain of the sample material. The final result of this experiment

activity is to give the identity or the data of the material which is the structural properties of

crystalline materials. As the result the unknown material sample is ZnO (Zinc Oxide) BCC crystal

structure with 36,4169 deg As highest peak intensity and 0,1487 deg, FWHM with the grain size is

56,24 nm and strain of the material is −4,277× 10− 4. The result of the analysis did not always give

the 100% same graph as compared with the database, the graph shifted or the intensity peak was

wider. It identifies that there is a certain factor that can be affecting that. To minimize that, the

instrument needs to be calibrated frequently.

INTRODUCTION
In the material science engineering field, there are many techniques to define or characterize the

material, starting from surface analysis to atomic analysis. X-ray Diffraction is the one method to

characterize the material also known as the non-destructive test method. X-ray Diffraction (XRD) is

also the best way to characterize crystalline materials with a non-destructive engineering method.
With this method, we can define the structure, phase, crystal orientations, grain size, strain, and

crystal defects [1]. Before discussed deeply regarding X-ray diffraction, first need to know about

the basic principle used in X-ray diffraction is X-ray and the diffraction. X-rays are electromagnetic

waves with a wavelength of 0.1 – 10 (amstrong) or the equivalent of the atomic distance in the

matter [2]. Many sources of the X-rays, commonly The source for X-ray in XRD Machine is using
Cu λ Kα 1 (Copper). The working principle of XRD testing is that when a material is subjected to X-

rays, the intensity of the transmitted light is lower than the intensity of the incident light. This is due

to absorption by the material and also scattering by the atoms in the material. Some of the scattered

X-ray beams cancel each other out because the phases are different and some also reinforce each

other because the phases are the same. X-ray beams that reinforce each other are called diffraction

beams, the detail of the different of interferences see Figure 1.

Figure 1. (a) Constructively Interference, (b) Destructively Interference.[ 5 ]

The diffraction happened when two waves are mutually reinforce (or constructively interfere with)

one another. When X-rays hit a solid material, the rays will be scattered in various directions due to

the electrons contained in the atom. The Bragg’s Law shown or represented that concept by this

formula : Brag g ' s Law →=2 dsin . When X-rays hit a solid material, the rays will be scattered in

various directions due to the electrons contained in the atom as shown in figure 2. [5]
 Figure 2. Diffraction of X-ray by plane of atoms.[ 5 ]

This Bragg's law is a basic method for the XRD, which is applied to the XRD system machine. The

application of this theory in common ways by using powdered specimens or what is usually called

polycrystalline which are fine particles and also when given monochromatic x-ray radiation they

will be randomly oriented. and each grain or what is usually called a crystal has a different

orientation and some are oriented correctly so that there are several possibilities for the

crystallographic plane to be ready for the diffraction process. To determine the angle at which the

diffraction process occurs in powder specimens, you can use a tool called a diffractometer.

OBJECTIVES
1. Understanding the main components of X-ray Diffraction

2. Defining the main principle of X-ray Diffraction

3. Determining the material that is crystalline or amorphous

4. Determining the material of the unknown sample by clarifying the graph from the experiment

with the database.

5. Calculating the crystal size of the material and the strain of the material

EXPERIMENTAL WORK

a. Instrumentation

Figure 1. Rigaku Mini Flex II .[ 3 ]

A. X-Ray Tube

The X-Ray Tube produces electrons. A tungsten filament is the cathode and also there is the

anode inside an x-ray tube. The cathode is heated so that some electrons have enough energy to

escape from its surface.

B. X-Ray Source

The X-Ray source commonly uses Cu (Copper) to produce Cu-K

C. Sample Holder

For sample plates made from glasses. There is a difference between sample plates for the bulk

sample and powder sample. The important thing is the sample holder can be adjusted

horizontally and vertically to maximize the diffraction process of the material and the X-ray at

different angles. This sample holder was cleaned before being used to prevent impurities from

distracting on the analyzed process and affecting the final result.

D. Detector
 A device that receives and records the diffraction that occurs as the X-ray hits the material

sample. The type of detector is determined by the sensitivity and resolution desired.

E. Chiller

The chiller's temperature, which is around 18-20 degrees Celsius, is used to cool the anode in

the X-Ray tube. The fluid that is used in the system is water with some addition of chemicals.

F. XRD Software

After the experimental process which is a whole process of X-ray diffraction to the sample

material, the recorded data was shown as a graph and diffraction degree in the table and then

continued to be analyzed by the following software or applications: PDXL2, PDF-2 Release

2022, and Standard Measurement Software.

b. Preparing a Sample for Analysis
Prepared the sample (unknown material) and the sample holder. The sample that was used was

powder-shaped. The sample holder was cleaned with distilled water or solvent to remove any

residual or impurities. Ensure the sample holder is already clean and dry then put the sample

material on it and distribute it to all the areas of the holder. Pressing gently with a glass plate to the

sample until it has both a flat surface and uniform spread. Placed the prepared sample into the

diffractometer and closed the door of the XRD machine until the light door was turned on it

identified is the door was closed properly. Turn on the chiller for the cooling system until they are

ready. Then sample material is ready for X-ray Diffraction data recording.
c. Characterization Process
The sample “MSE 503-03” was ready in the diffractometer. To run the diffraction process utilizing

through three distinct applications which are PDXL2, PDF-2 Release 2022, and Standard

Measurement Software. For setting parameters of the diffraction such as Angular angle (θ) and

setting scan speed used the standard measurement software. The angular angle that was set between

30° and 60° and for scan speed is 4 minutes/degree. So, the total duration of scanning time was

approximately 7.5 minutes. After the scanning or diffraction process was finished the result data

was recorded and shown as a diagram (intensity vs 2θ) and the table of 2θ. The result data

compared with the database material using PDF-2 released in 2022 to identify what is the structure

of the material based on the the 2θ and intensity.

RESULTS AND DISCUSSIONS
A. Determining the material of the unknown sample
After comparing the data results with the database from the PDF-2 released in 2022, found that

the 2-theta vs Intensity of the unknown material was matched to the 2-theta vs Intensity of the

Zinc Oxide (ZnO) material. The result showed similar with the material Zinc Oxide (ZnO). So,

the unknown sample is ZnO. Based on the The graph (figure 2) can be matched with the

unknown graph.

1.2e+004
Meas. data:unknown MSE503

1.0e+004

8.0e+003
Intensity (counts)

6.0e+003

4.0e+003

2.0e+003

0.0e+000
20 30 40 50 60
2-theta (deg)

Figure 2. XRD Graph from Standard measurement software

The graph shows some information mainly the graph shows the relationship between intensity

versus 2θ angle. Following the setup (scanning speed and angle range) that was conducted in the

diffraction is 10 minutes measurement. In the first 3 minutes (2θ = 30 deg), there are no

significant peaks in the graph, however when 2θ = 31,9477 the peak starts to come out. There

are 3 very significant peaks in the range 30 deg – 40 deg, which are peaks in 2θ = 44,589 deg

and the highest peak in 2θ = 36,4169 deg . and also subsequent peaks were observed at 2θ =

47.675 degrees, and 2θ = 56.7053 degrees. Based on the database, the material with those peaks

can identified as ZnO. The XRD graph below shows the result recorded from another
 experiment with the same result which is ZnO. (Figure 3)

Figure 3. The X-ray diffraction pattern of the result from the experiment [4]

B. Calculating Crystal Size by the Sherrer Equation

Based on the data result of the diffraction process the intensity graph of the peak has a width

instead sharp shape. It shows the graph of ZnO not only shows the intensity but also defines the

crystal size of ZnO using the peak position (2) table. To determine the size using the Scherrer’s

9
equation grain¿ (t¿)= B 1 . The peak position (2) = 36,4169 deg, FWHM (2) = 0,1487
cos
2

deg, and Cu λ Kα 1 = 0,154056 nm. After calculating, the grain size is 56,24 nm as shown in the

table down below :

No. 2-theta d Height FWHM Int. I Int. W Asym.

(deg) (ang.) (counts) (deg) (counts deg) (deg) Factor
 1 31.9477(19) 2.79900(16) 5191(72) 0.1519(16) 1061(4) 0.204(4) 1.68(9)

2 34.589(2) 2.59105(16) 3820(62) 0.148(2) 753(4) 0.197(4) 1.51(10)

3 36.4169(18) 2.46510(12) 9080(95) 0.1487(17) 1810(7) 0.199(3) 1.47(7)

4 47.675(2) 1.90595(9) 2168(47) 0.145(3) 423(3) 0.195(6) 1.29(9)

5 56.7053(17) 1.62200(5) 3484(59) 0.1423(18) 664(4) 0.191(4) 1.25(7)

Tabel 2. Data of ZnO Diffraction

 Peak Position ( 2θ )=36,4169 deg

 FWHM ( 2 θ )=0,1487 deg

 Cu λ Kα 1 = 0,154056 nm

 Crystal ¿ (t¿)=5 6 ,24 nm

C. Determining strain

Another factor that influences the width shape of the intensity graph is residual stress at the ZnO so

according to that phenomenon using the XRD characterization is also an effective tool to examine

residual stress in solids, by the William-Hall method, can calculate the estimation of the strain

based on the peak position (2) table. However, we must use the conversion to change degrees to

radians which is 1 deg= deg π as the detail shown on down below :

180 deg

Peak position Peak position FWHM β cosθ 4 sinθ

2θ (°) θ (°) β (°) (rad) (rad)
31,9477 15,97385 0,1519 0,002547598 1,100250883
34,589 17,2945 0,148 0,002465171 1,188548456
36,4169 18,20845 0,1487 0,002464228 1,249287884
47,675 23,8375 0,145 0,002313887 1,615804467
56,7053 28,35265 0,1423 0,002184861 1,898705223

Tabel 3. Data of β cosθ vs 4 sinθ for measuring strain

 0.0026

0.0025 f(x) = − 0.00042770330229558 x + 0.00299843287428376

0.0024
β cos θ

0.0023

0.0022

0.0021

0.002
1 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2

4 sin θ

Figure 4. The graph of β cosθ vs 4 sinθ.

So, we can find strain from the slope y=−4,277 ×10−4 x+ 2,988× 10−3

−4
ε =−4,277 × 10

CONCLUSION
Characterization of material using X-ray Diffraction was a very important and useful method. By

this method can identifying materials, crystal structure, lattice parameter, crystallite size, and strain.
In this experiment concluded that The XRD results show the unknown sample (MSE 503-03) was

Zinc Oxide with crystal structure Body Center Cubic (101), crystalline size of 56,24 nm and strain

of the material is 4,277.

REFERENCES

[1] Andrei A. Bunaciu, Elena gabriela Udriştioiu & Hassan Y. Aboul-Enein (2015) X-Ray

Diffraction: Instrumentation and Applications, Critical Reviews in Analytical Chemistry, 45:4, 289-

299, DOI: 10.1080/10408347.2014.949616

[2] Oliver H. Seeck, Bridget Murphy. (2014) X-Ray Diffraction: Modern Experimental
Techniques, Number-13 : 978-981-4303-60 , New York
[3] Al Ashraf, Adullah. Nitrogen And Sulfur–Doped Carbon Nanofiber Mixed Oxides Composites

For Supercapacitor Applications. 2016

[4] Mendes, Carolina & Dillari, Guilherme (2022) Antibacterial action and target mechanisms of
zinc oxide nanoparticles against bacterial pathogens, Nature Scientific report 12:2658, DOI:
https://doi.org/10.1038/s41598-022-06657-y

[5] Calister, Wiliam D and Rethwisch David G (2014) Material Science and Engineering:

Introduction, ISBN: 978-1-118-32457-8 , USA