Material Science and Solid State Laboratory (Experiment

8) 2015

Faculty of Industrial Science and Technology

Material Technology Programme
MATERIAL SCIENCE & SOLID STATE LABORATORY
(BSP 2422)
Semester 1 2015/2016

Title of Experiment: X-Ray Structural Analysis

Date of Experiment: 4th November 2015
Date of Submission: 19th November 2015
Instructors Name : En Halim bin Paboh

Group of Member

Name

ID

1. NADIA SABRINA BINTI MOHAMAD AZMI

SC14013

2. LAU PUI PUI

SC14036

3. TAN YI JIE

SC14041

4.
5.
Group No.

: 6

Section

: 01G

Marks
Part A
Part B
TOTAL

:
55
45
100

Material Science and Solid State Laboratory (Experiment

8) 2015

FACULTY OF
INDUSTRIAL
SCIENCE AND
TECHNOLOGY
INDUSTRY
Experiment 1: X-Ray Structural Analysis
NADIA SABRINA BINTI MOHAMAD AZMI
SC14013
LAU PUI PUI
SC14036
TAN YI JIE
SC14041
Universiti Malaysia Pahang,
Lebuhraya Tun Razak
26300 Kuantan
Pahang Darul Makmur
Tel.:09-5492501, fax: 09-5492544
E-mail: yytan996@gmail.com
Submitted: 19th November 2015

Abstract: This experiment is X-ray structural analysis. The purpose of conducting this
experiment is to use of X-ray diffraction techniques for investigating various types of crystal
structure encountered in metallic materials. Theoretically, X-ray diffraction techniques are a very
useful characterization tool to study non-destructively, the crystallographic structure, chemical
composition and physical properties of metallic and ceramic materials. Besides, it can also be
used to measure various structural properties of these crystalline phrases such as strain, grain
size, phase composition and defect structure. X-Ray diffraction is also used to determine the
thickness of thin films as well as the atomic arrangements on various planes within the structures.
Three basic crystal structures encountered in metallic materials are the Body-Centered Cubic
(CFC), Face-Centered Cubic (FCC) and Hexagonal Close-Packed (HCP).
Keywords: X-ray diffraction, crystallographic, metallic, ceramic, crystalline, grain, thin film, BodyCentered Cubic, Face-Centered Cubic, Hexagonal Close-Packed

1. Introduction
X-ray crystallography is a tool used to identify
the atomic and molecular structure of a
crystal, in which the crystalline atoms cause a
beam of incident X-rays to diffract into many
specific directions. By measuring the angles
and intensities of these diffracted beams, a
crystallographer can produce a three-

dimensional picture of the density of electrons

within the crystal. From this electron density,
the mean positions of the atoms in the crystal
can be determined, as well as their chemical
bonds, their disorder and various other
information. Crystals are regular arrays of
atoms and X-rays can be considered waves of
electromagnetic radiation. Atoms scatter Xray waves, primarily through the atoms'

Material Science and Solid State Laboratory (Experiment

8) 2015

electrons.

Figure 1: The reflection of X-ray beam by the (hkl)

planes of a crystal. No reflected at an arbitrary angle of
incidence.

Figure 4: Sample output

2. Materials and method

2.1 Apparatus and material
The apparatus needed for this experiment
is Rigaku Miniflex XRD machine.
The material needed for this experiment is
commercial sample (titanium dioxide).

Figure 2: At the Bragg angle, the reflected rays are in

phase and reinforce one another.

Figure 3: Schematic representation of the in-phase

condition.

A regular array of scatters produces a regular

array of spherical waves. Although these
waves cancel one another out in most
directions through destructive interference,
they add constructively in a few specific
directions, determined by Bragg's law:
n = 2d sin
Here d is the spacing between diffracting
planes, is the incident angle, n is any integer,
and is the wavelength of the beam. These
specific directions appear as spots on the
diffraction pattern called reflections. Thus, Xray diffraction results from an electromagnetic
wave (the X-ray) impinging on a regular array
of scatters (the repeating arrangement of
atoms within the crystal).

2.2 Method
1. The apparatus is set up as shown in the
figure below.
2. Prepare the sample used.
Titanium dioxide, TiO2 was put into
the slide. Wear the gloves while
preparing the slide.
3. Make sure the slide is all occupied
evenly by titanium dioxide, TiO2.
4. Remove excessive powder by using
tissue paper.
5. Slowly insert the sample into the XRD
machine.
6. Wait the sample approximately one
hour, and then take it out and record
the result.
7. The results are recorded in the graph
and table below.

Figure 5: X-ray Diffraction machine

Material Science and Solid State Laboratory (Experiment

8) 2015

Pea
k

1
2
3
4
Figure 6: Automatic voltage regulator and cooler
attached with X-ray diffraction machine

3. Result

5
6
7
8
9
10
11
12

Graph 1: The graph of intensity of the diffracted beam

against diffraction angle 2

The following equations were used to count dspacing and lattice parameter.
=2 dsin ---------- eq.1

d=
----------- eq.2
2 sin
given that =1.5418
a
d=
2
h +k 2+ l2
a = d h2 +k 2 +l 2 -------- eq.3

13
14

Relativ
e
intensit
y

sin

25.36
3

3495

0.22
0

36.98
8

200

37.83
6

743

38.61
3

225

48.07
0

1040

53.92
2

615

55.09
5

630

62.15
6

108

62.71
5

492

68.79
6

212

70.34
4

225

74.09
0

16

75.09
4

346

76.05
9

96

hkl

Lattice
parameter
, a ()

(101
)

4.955

3.504

0.31
7

(103
)

7.691

2.432

0.32
4

(004
)

9.516

2.379

0.33
1

(112
)

5.705

2.329

0.40
7

(200
)

3.788

1.894

0.45
3

(105
)

8.673

1.701

0.46
2

(211
)

4.088

1.669

0.51
6

(213
)

5.590

1.494

0.52
0

(204
)

6.632

1.483

0.56
5

(116
)

8.408

1.364

0.57
6

(220
)

3.784

1.338

0.60
2

(107
)

9.058

1.281

0.60
9

(215
)

6.934

1.266

0.61
6

(301
)

3.956

1.251

dspacing,
d
()

Table 2: Various data about the peak

1. The highest peak is (101), followed by

(200) and (004).
2. To determine the structure of crystal, take
the sum of h, k and l.
( h+k + l )=( 1+0+1 )=2
Since the sum of h, k and l is an even
number, thus the structure is a BCC
structure.

Material Science and Solid State Laboratory (Experiment

8) 2015

4. Lab Requirements
1. [1 1 1] denoted the direction and (1 1
1) denoted to a plane. <1 1 1> is the
family of directions and {1 1 1} is the
family of planes.
2. The inter-planar spacing, d for sets of
{1 2 1} planes in iron, where a =
0.2865nm.
a
d h kl = 2 2 2
h +k +l
0.2865 nm
2 2 2
1 +2 + 1
0.1170 nm
3. The angle where iron diffracts Cu-K
X-rays of wavelength 0.1541 nm.
n=2 dsin
n
sin =
2d
1(0.1541nm )

2(0.1170 nm)
0.6585
=41.19
4. The lattice parameter for BCC iron.
4 R= 3 a
4R
a=
3
4(0.1241nm)

3
0.2866 nm
5. (1 1 1) plane in a FCC unit cell

6. (1 1 0) plane in a BCC unit cell

5. Discussion
The schematic of X-ray apparatus is shown as
below.

Figure 2: Schematic of X-ray apparatus

From the experiment, the values of 2 for

some of the peaks were obtained to be 25.36,
36.99, 37.84, 38.62, 48.07, 53.92, and
55.10.
The Miller indices found for each peak was
(101), (103), (004), (112), (200), (105) and
(211) respectively.
The d-spacing was also calculated to be
3.504, 2.432, 2.379, 2.329, 1.894,
1.701 and 1.669 respectively.
There were some errors during carry out the
experiment. One of the errors was that the
Titanium dioxide (Ti O2 ) powder was not
spread evenly and there may be dents or holes
on the surface of the powder which may
influence the reading obtained. Beside this,
powder may contaminate with impurities such
as dust and small insects.
Several precautions that can be taken to avoid
the error occur are to ensure that the machine
does not emit any strange odor, the door of the
Rigaku Miniflex XRD machine must also be
close tight when the experiment is being
carried out. Furthermore, the procedure in the

Material Science and Solid State Laboratory (Experiment

8) 2015

lab manual and instruction of lab instructor

must be followed.

a=d

To improve the experiment, the suggestion for

this experiment is to change the titanium
dioxide (Ti O2 ) powder every so often to
avoid having contaminants in the powder.
Other than this,the safety operation of
equipment must be ensured by checking the
condion of the Rigaku Miniflex XRD machine
regularly.

=4.955

6. Conclusion
In conclusion, the highest peak was (101),
followed by (200) and (004). The crystalline
structure of Titanium oxide (Ti O2 ) was
body centered cubic structure (BCC).
7. Acknowledgement
A token of appreciation to Dr Rasidi bin
Roslan and the laboratory assistants for all the
guidance in the process of completing this
journal. Not forgetting all my group members
whom give full commitment in conducting the
experiment and completing this journal.
8. Reference
[1] Bavarian lab, X-ray Structural Analysis,
2014.
[2] Frederic P. Miller, Agnes F. Vandome,
John McBrewster (2010), Braggs Law
9. Appendix
Calculations
For peak (101)
From eq 2:

d=
2 sin
given that =1.5418
1.5418
d=
2(0.220)
=3.504
From eq 3:

h2 +k 2 +l2
=3.504 12+0 2+1 2

For peak (103)

1.5418
d=
2(0.317)
=2.432
a=d h2 +k 2 +l 2
=2.432 12+0 2+ 32
=7.691
For peak (004)
1.5418
d=
2(0.324)
=2.379
a=d h2 +k 2 +l 2
=2.379
=9.516

02 +02 +4 2

For peak (112)

1.5418
d=
2(0.331)
=2.329
a=d h2 +k 2 +l 2
=2.329
=5.705

12+12 +22

For peak (200)

1.5418
d=
2(0.407)
=1.894
a=d h2 +k 2 +l 2
=1.894
=3.788

2+ 02 +02

For peak (105)

1.5418
d=
2(0.453)
=1.701
a=d h2 +k 2 +l 2
=1.701
=8.673

12+0+ 52

Material Science and Solid State Laboratory (Experiment

8) 2015

For peak (211)

1.5418
d=
2(0.462)
=1.669
a=d h2 +k 2 +l 2
=1.669
=4.088

22+12 +12

For peak (213)

1.5418
d=
2(0.516)
=1.494
a=d h2 +k 2 +l 2
=1.494
=5.590

22+22 +0 2

For peak (107)

1.5418
d=
2(0.602)
=1.281
a=d h2 +k 2 +l 2
=1.281
=9.058

12+0 2+7 2

For peak (215)

1.5418
d=
2(0.609)
=1.266
a=d h2 +k 2 +l 2
=1.266
=6.934

22+12 +52

22+ 0+4 2

For peak (116)

1.5418
d=
2(0.565)
=1.364
a=d h2 +k 2 +l 2
=1.364
=8.408

=1.338
=3.784

22+12 +32

For peak (204)

1.5418
d=
2(0.520)
=1.483
a=d h2 +k 2 +l 2
=1.483
=6.632

For peak (220)

1.5418
d=
2(0.576)
=1.338
a=d h2 +k 2 +l 2

12+12 +6 2

For peak (301)

1.5418
d=
2(0.616)
=1.251
a=d h2 +k 2 +l 2
=1.251
=3.956

32+ 02 +12