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X-ray Diffraction (XRD) of Magnesium Oxide, MgO

Muhammad Amir Akmal Bin Adnan, Nurul Syahirah Binti Zakaria, Norsyazana Ain Binti
Ab Aziz, Zulaikha Binti Zulkifli, Mazidah Binti Zakaria ,Zainil Husni Bin Ahmad Zinon,

Metallurgical Engineering (RK-56) MBM2, University Malaysia Perlis (UniMAP)

Qualitative analysis using X-Ray Diffraction technique was conducted by using XRD 6000,
Shimadzu X-Ray Diffractometer in order to identify the phases present in this experiment. The
lattice parameter of chromium was calculated by using analytical method and Expert High Score
Plus has been used to run analysis of the sample given.

1.0 Introduction
The phenomenon when the atomic planes of a crystal cause an incident beam of X-rays to
interfere with one another as they leave the crystal is called X-ray diffraction(XRD). XRD is
used for the study of atomic spacing and crystal structures [1]. It is based on constructive
interference of monochromatic X-rays and a crystalline sample. These X-rays are generated by
cathode ray tube, filtered to produce monochromatic radiation, collimated to concentrate, and
directed toward the sample [1].When conditions satisfy Bragg's Law the interaction of the
incident rays with the sample produces a diffracted ray and constructive interference. This law
relates the wavelength of electromagnetic radiation to diffraction angle and lattice spacing in a
crystalline sample [1].XRD is used widely for identification of unknown crystalline materials,
characterization of crystalline materials and measurement of sample purity also determination of
unit cell dimensions. The calculation of XRD technique involved the Braggs Law [1].
The incident angle is considered equal to reflected angle in phases of beam. Ray of incident
beam is in phase and parallel to the point the top beam strikes the top layer atom Z. The second
beam continues to next layer where it scattered by atom B it must travel the extra distance
AB+BC if the two beams are to continue travelling adjacent and parallel. This distance must be
an integral (n) multiple of wavelength () for phases of two beams to be same [2].

(1) n =AB+BC
Recognizing d as hypotenuse of right triangle Abz, use trigonometry to relate d and to distance
(AB+BC).Distance AB is opposite so,
(2) AB=d sin
AB=BC equation (1) becomes
n =2AB
Substituting equation (2) in (3)
(4) n =2d sin

Braggs Law is derived. Where n is an integer determined by the order given, is the wavelength
of x-rays, d is the spacing between the planes in the atomic lattice, and is the angle between the
incident ray and the scattering planes [2].
Crystal structure is one of the most important aspects of materials science and engineering as
many properties of materials depend on their crystal structures. In the cubic system planes and
directions having same indices are perpendicular to each other .There are examples of elements
in cubic lattices which are iron and sodium chloride. Crystal structures for cubic lattices have
three types which are simple cubic, body-centered cubic and face-centered cubic [3].
To determine the crystal structures for cubic lattices there are some criteria which must be
known. For example number of atoms in the unit cell, distance between atoms (d), atomic
packing factor (APF) and coordination number [3]. Number of atoms in unit cell for FCC are 4
while BCC is 2.The atomic packing factor for FCC is 0.74 while bcc is 0.68 and cubic structure
is 0.52.The coordination number for FCC is 12 while BCC is 8 and simple cubic is 6 [3].

For powder sample we use the aluminium sample holder. The aluminium sample holder had to
be cleaned first using acetone. This step is must to clean the sample holder from the impurities.
Next, the powder is poured into the sample holder. After that the powder is pressed using the
glass slide, until the powder become flat. This step is to ensure the powder is fully filled in the
sample holder. Then the excess powder is remove with slide the glass slide along the sample
holder surface. This step is necessary to ensure x-rays is diffracted evenly. After that, the sample
holder is hold 45 to ensure that the powder is not spilling out from the holder. Finally, the
sample holder is insert into the diffractometer to be analyze. The scan range is between 10
to 70 .


The magnesium (Mg) was detected by using X-ray Diffraction(XRD) method. By doing XRD
analysis, the XRD pattern can be obtained.

Figure 4.1 XRD pattern of Mg

Figure 4.2 XRD pattern of Mg

XRD analysis can be analyzed by using mathematical method and database of HighScore Plus
software. Figure 4.1 shows the XRD pattern of Mg powder using the software. The highest
peaks of Mg were identified from this XRD analysis. The result in the database of HighScore
Plus software with Pattern Diffraction File ( PDF) were used to search and match technique.
The highest peak of Mg can be detected in the range at 2 = 10 to 80. Referring to the pattern,
the higher peak means it has higher intensity and high intensity means more photons were
collected [1].
From the XRD pattern, magnesium crystallographic parameters can be obtained. The result were
shown in Table 4.1 and Table 4.2.
Table 4.1 The highest peak of Mg
There are five peaks at 21 = 34.4385, 22=36.7432, 23=47.7415,
24= 62.9810 and 25=68.6756 with intensity 6348.52, 2614.21, 709.20,
941.52 and 462.87 have been found in the XRD pattern which are related to
the Mg.
Table 4.2 XRD results and crystallographic data of Mg
Compound name
Reference code
Chemical formula
a ()
b ()
c ()
Alpha ( )
Beta ( )
Gamma ( )
Crystal system
The Mg peaks shows that the Mg powder

Zinc oxide
have a hexagonal crystal structure as the

crystallographic parameters that is a = b c which are 3.2094=3.20945.2112 [2].

X-Ray Diffraction (XRD) is a scattering of X-Rays by the atom of a crystal that produces an
interference so that the diffraction pattern gives information on the structure of the crystal or
identity of a crystalline substance. From our observation we found that Magnesium (Mg) has
been successfully analysed and identified the unknown crystalline materials. As a conclusion we
found that Magnesium powder is a hexagonal crystal structure.

[1] B. L. Dutrow, L. State, C. M. Clark, and E. Michigan, "X-ray powder diffraction (XRD),"
Techniques, 2016. [Online]. Available:
http://serc.carleton.edu/research_education/geochemsheets/techniques/XRD.html. Accessed:
Nov. 29, 2016.
[2] "X-ray diffraction, Braggs law and Laue equation - MSE 5317,". [Online]. Available:
http://electrons.wikidot.com/x-ray-diffraction-and-bragg-s-law. Accessed: Nov. 29, 2016.
[3] "Introduction to Material Science,Chapter 3,The structure of Crystalline Solid,". [Online].
Available: http://web.utk.edu/~prack/mse201/Chapter%203%20structure.pdf. Accessed: Nov. 29,