Professional Documents
Culture Documents
Assignment No.1 Group-5 Mat-13a
Assignment No.1 Group-5 Mat-13a
1
Table of Contents
Abstract: ........................................................................................................................................ 3
Introduction: ................................................................................................................................. 4
Scanning Electron Microscopy: ................................................................................................... 5
Energy Dispersion Spectroscopy: ................................................................................................ 6
X-Ray Diffraction: ........................................................................................................................ 9
Indexing of the Peaks ................................................................................................................ 10
Indexed Pattern of MoSi2 .......................................................................................................... 11
Unit Cell of MoSi₂ .................................................................................................................... 12
Conclusion: .................................................................................................................................. 12
References:................................................................................................................................... 13
2
Abstract:
Molybdenum Disilicide, a refractory ceramic shows better properties at high temperature than pure
Molybdenum. In this assignment we have discussed the characterization of MoSi2 using different
and X-ray diffractometry we have identified the grain morphology, chemical composition, and
3
Molybdenum Disilicide Characterization
Introduction:
There are many types of materials that fall into the category of refractory metals and molybdenum
is one of them. It has a high melting point about 3000°C but when heated to that high temperature
it makes an oxide, which is called Molybdenum Oxide (MoO) which has a very low melting point
(595°C) as compared to that of pure metal. This formation of oxide makes Molybdenum unsuitable
Those metal oxides are better which have high melting point than the base metal. To overcome
this problem, Molybdenum is reacted with different materials. Molybdenum, when reacts with
silicon makes 2 intermetallic compounds, MoSi2 and Mo5Si3. MoSi2 is prepared by Self
propagating high temperature synthesis (SHS) which is followed by crushing in a planetary ball
mill for 5 h with a rotational rate of 200 rpm and a ball to powder weight ratio of 5:1. The SHS
powder was processed by spray drying processing followed by heat treatment processing at
1300°C in vacuum environment for 1 hour. Now, this powder was used as spray material.[1]
Now, we are going to characterize this ceramic powder using 3 different characterization
techniques. These techniques include Scanning electron microscopy (SEM), Energy dispersive
spectroscopy (EDS), and X-ray diffractometry (XRD). All three techniques give us different
details about the powder sample. Scanning electron microscopy helps us identify the morphology
of the powder sample. Energy dispersive spectroscopy gives us the composition of elements in
different phases in the microstructure of the powder sample while XRD helps us identify the crystal
4
Scanning Electron Microscopy:
Scanning electron microscopy is a powerful tool for the characterization of the materials. It is a
non-destructive type of testing with versatile modes of operation. This technique uses the high
energy electron beam to focus on the sample of interest, which results in several interactions that
The images above show the spherical shape of the powder particles. Image a show spherical shape
of the particles and with least magnification, i.e., about 100 microns while b shows more magnified
image i.e., 25 microns and c with the highest magnification (about 5 microns). As the powder was
5
prepared by spray drying technique, which produces near spherical particles that’s why their shape
is spherical. Spherical morphology of particles leads to better flow rate with high deposition
efficiency. [1]
Moreover, it gives us the information that a ceramic made up of powder which has approximately
same shape and size tends to give us better properties in the application. The image below shows
In EDX systems, which are connected to electron microscopy equipment (SEM or TEM), the
microscope's imaging capabilities detect the specimen of interest. The peaks in the spectra
produced by EDX analysis correspond to the components that make up the true composition of the
There are two images that are shown below for explaining the composition of different phases.
First image is the BSE (back scattered electron) image, which shows the presence of different
6
phases in the microstructure. While the second image shows compositions of different elements in
The dark phase A shows only one phase that is MoSi2 phase. Whereas the second phase B shows
a mixture of Mosi2 and Mo5Si3 phases. It includes about 0.69 mol% MoSi2 while 0.31% Mo5Si3.
The other two light phases i.e., C and D also show a mixture of MoSi2 and Mo5Si3 phases, but both
have different ratios or mol percent of MoSi2 and Mo5Si3. Thus, the darker phases have more
MoSi2 present than the light phases, where the mixture of phases is present. Also, the percentage
7
Figure 4 EDS spectrum of MoSi2 powder
Phases MoSi2/Mo5Si3
B 2.225
C 3.19
D 4.45
From the table above, we can see that phase A contains 100% MoSi2, while in the other phases
8
X-Ray Diffraction:
Now the last step in characterization of the powder is to determine the crystal structure whether it
is BCC, FCC, HCP or Tetragonal because each crystal structure type has its specific properties.
The X-ray diffraction (XRD) technique mainly gives us the information about the crystal structure
of the element/powder. In this technique x-rays hits on the powder particle and it will diffract the
rays in some specific angles which ultimately gives us peak like pattern and then with the help of
indexing we can find the crystal structure of the powder. As we know that Mo is the refractory
ceramic and often used in applications where high strength at high temperature is the primary
requirement.
hexagonal form (β-MoSi2) [2]. MoSi2 is most interesting industrially for its excellent oxidation
Figure 5 X-ray diffraction pattern of MoSi2 and Mo5Si3 phases (λ-Cu Kα) after Si reaction with Mo at 1530◦ C, 3 min
9
In the manufacturing of MoSi₂, its different intermetallic compounds are also produced so it is
very critical to recognize the degree of purity of MoSi₂ with the intention to manage the residences
of heating elements. Powder XRD technique is appropriate to quantify MoSi₂ purity since it can
clearly differentiate MoSi₂ from other Mo-Si intermetallic compounds. If detailed crystal structure
information is not available for the materials you want to analyze, you could use structureless
10
Indexed Pattern of MoSi2:
The (h, k, l) values comes from the indexing of the pattern shows the Tetragonal crystal
structure of MoSi2.
11
Unit Cell of MoSi2:
The structure is a long-range ordered crystal structure made through stacking 3 bcc lattices
alongside the c axis, as shown in Fig. 8. This unique crystal structure is thought to be responsible
for the anisotropy that is frequently associated with MoSi2. For example, compression tests on
MoSi2 single crystals at elevated temperatures showed that the dominant primary slip planes are
the {1 1 0} planes although slip on the {0 1 3} planes was also observed [4]. At approximately
Conclusion:
In ceramic industry even a small single mistake leads to the failure of the final product that’s why
during the fabrication process, we have to carefully control all the parameters. If all the parameters
are carefully controlled, the processing will be efficient. Powder characterization, Purity, Particle
size, Particle size distribution, Reactivity, Viscosity are some factors on which our ceramic
12
material production necessarily based. In this report we have discussed the different Powder
Characterization Techniques by using the Molybdenum Disilicide powder, which shows us the
shape, composition, and crystal structure of the MoSi2. This information is very important to be
considered while making something from the powder, so you don’t have to put too much effort for
the better result, by knowing this information (Powder Characterization) one can predict and use
References:
[1] Y. Wang, D. Wang, J. Yan, and A. Sun, “Preparation and characterization of molybdenum
disilicide coating on molybdenum substrate by air plasma spraying,” Applied Surface
Science, vol. 284, pp. 881–888, Nov. 2013, doi: 10.1016/j.apsusc.2013.08.029.
[3] Structureless whole powder pattern fitting analysis of MoSi₂. (n.d.). Rigaku.com.
Retrieved April 17, 2022, from https://www.rigaku.com/pt-br/node/603
[4] Jeng, Y.-L., & Lavernia, E. J. (1994). Processing of molybdenum disilicide. Journal of
Materials Science, 29(10), 2557–2571. https://doi.org/10.1007/bf00356804
13