LABORATORY REPORT

MST 613

EXPERIMENT NO 2
EXPERIMENT TITLE X-Ray Diffraction (XRD)
Technique
NAME Nur Fadhlina Binti Bisahari
STUDENT ID 2017428094
GROUP AS2305M2
SUBMISSION DATE 15 October 2019
LECTURER’S NAME Dr. Mohd Muzamir Bin Mahat
OBJECTIVE

1. To observe method of evaluating crystalline structure by using x-ray diffraction.

2. To understand the use of Bragg’s Law and its relation to crystal structure.

INTRODUCTION

X-ray diffraction (XRD) can be defined as an analytical technique that has been widely used for
phase identification of a crystalline material and they have been identified to provide information
on unit cell dimensions. The analyzed material is finely ground, homogenized, and average bulk
composition is determined.
The picture above shown one of the XRD that has been used at Faculty of Applied Science,
UiTM Shah Alam. X-rays are generated by a cathode ray tube, filtered to produce
monochromatic radiation, collimated to concentrate, and directed toward the sample. The
interaction of the incident rays lead to Bragg’s Law:

n x wavelength = 2dsin (theta)

INSTRUMENTATION

An X-ray source was required in this experiment, the sample under investigation and a detector
picked up the diffracted X-rays. The X-ray most commonly used is that emitted by copper,
which wavelength for the K radiation is = 1.5418A. Diffraction occurred in every possible
orientation of 2theta when the incident beam strikes a powder sample. The diffracted beam may
be detected by using a moveable detector such as Geiger counter, which is connected to a chart
recorder.

PROCEDURE

1. Two (named as X and Y) samples was obtained from your instructor, placed it onto the
double-side tape which is then placed on an aluminium sample holder, a powder sample
was prepared and a spatula was used to spread the powder onto the double-side tape.
2. The instructions for the Xpert-Pro X-ray diffractometer was read, which are on the wall
above the instrument.
3. The instrument was set at optimum setting as followed:
time constant 2
range ?
chart speed: low
4. The sample holder was slide in and adjusted the beginning 2theta at 70 degree (It scans
from high degrees to low degrees)
5. The start knob and chart recorder (slow) was switched on simultaneously, the sample was
run on slow chart speed.
6. Stopped (switch start knob to off) and chart once scan gets down to 3 degree of 2theta.
Turned off X-ray.
7. All peaks on the chart was located and 2theta values corresponded and their values was
wrote into the data chart below. The necessary calculations was performed in the table
and the repeat distance in your unit cell was calculated.
8. The types of crystal structure was determined based on the pattern h,k,l.
RESULT

Sample 1:

2theta theta sin(theta) d=n x wavelength/2sin(theta) Find ( + + )=?

18 9 0.156 4.928 2.845

30 15 0.259 2.979 1.053
36 18 0.309 2.495 0.752
38 19 0.326 2.368 0.671
44 22 0.375 2.058 0.515
48 24 0.407 1.895 0.435
*Wavelength = 1.5418 A (0.15418 nm) for Cu Ka, assuming n=1 and a=0.564n
Sample 2:

2theta theta sin(theta) d=n x wavelength/2sin(theta) Find ( + + )=?

54 27 0.454 1.698 1.006

58 29 0.485 1.590 0.948
63 32 0.530 1.455 0.871
67 34 0.559 1.379 0.833
68 34 0.559 1.379 0.821
72 36 0.588 1.312 0.779
*Wavelength = 1.5418 A (0.15418 nm) for Cu Ka, assuming n=1 and a=0.564n
CALCULATIONS

Table 1:

2theta (30), a = 4.928 / √

= 2.845

2theta (34), a = 4.928 / √

= 1.053

2theta (36), a = 4.928 / √

= 0.752

2theta (38), a = 4.928 / √

= 0.671

2theta (44), a = 4.928 / √

= 0.515

2theta (48), a = 4.928 / √

= 0.435
Table 2:

2theta (54), a = 4.928 / √

= 1.006

2theta (58), a = 4.928 / √

= 0.948

2theta (63), a = 4.928 / √

= 0.871

2theta (67), a = 4.928 / √

= 0.833

2theta (68), a = 4.928 / √

= 0.821

2theta (72), a = 4.928 / √

= 0.779
DISCUSSION

Based from the experiment that has been carried out, the first sample was detected as Lithium
Manganese Oxide during the diffraction. As the 2theta (degree) increased, the value a that have
been calculated decreased as they going down below of the table. From Reference 1 result, the
three most reflections have the (1 1 1), (2 0 0), and (2 2 0) planes. We can determine the crystal
structure by using the Bragg’s equation. The sum of the h, k, l values of the intensity peaks of the
BCC crystal structure are all even.

The second sample known as Lithium Manganese Titanium Oxide. The result between the two
samples are quite the same. The 2theta of both sample almost had the same values. From our
graph, we can conclude the crystal structure based on the pattern h, k, l. Both samples has the
crystalline structure. The BCC and FCC crystal structure cannot be determined due to slight
errors during the experimental procedures.

The X-ray diffractions on both sample provided important data, which was then analyzed to
determine that the unknown sample is a Lithium Manganese Oxide and Lithium Manganese
Titanium Oxide. The experiment can be improved so that we can obtain more accurate and
consistent result. X-ray diffraction (XRD) can provide an analysis on crystalline structure and the
degree of crystallinity of materials. Besides that, they also can provide an information on
material quality.

In this experiment, we used the Bragg’s Law to explain the interference pattern of X-rays
scattered by crystals. The diffraction has been developed to study the structure of all states of
matter with any beam. The wavelength must be similar to the distance between atomic or
molecular structure. XRD can help to measure the average spacings between layers or rows of
atoms and they are also helps to determine the orientation of a single crystal or grain. XRD was
widely used in materials industry as they able to measure the size, shape and internal stress of
small crystalline regions. The most common benefits of XRD is they will help to determine the
crystal structure of an unknown material.
CONCLUSION

In my conclusion, we are able to observe and evaluate the atomic crystalline structure by using
x-ray diffraction. The objective was achieved as we finally understand the use of Bragg’s Law
and its relation to crystal structure. The structure of both sample is crystalline.

REFERENCE

1. X-ray Diffraction: XRD Services: EAG Laboratories. (n.d.). Retrieved from

https://www.eag.com/techniques/spectroscopy/x-ray-diffraction-xrd/.
2. Heiney, P. A. (n.d.). Retrieved from
https://www.physics.upenn.edu/~heiney/datasqueeze/basics.html.
3. X-Ray Diffraction: Instrumentation and Applications. (n.d.). Retrieved from
https://www.tandfonline.com/doi/abs/10.1080/10408347.2014.949616?scroll=top&need
Access=true&journalCode=batc20.