Institute of Space Technology

Department of Materials Science and Engineering

Ceramics lab (211409)
Assignment no.1
Section: MAT-13A

Submitted to Engr. Luqman Hashmi

Submitted by Group#5
Nawal Haider 200301055
Hassan Nadeem 200301054
Maaz Hassan 200301056
Rafay uz Zaman 200301052
Hamdan ur Rehman 200301050

Date of Submission 22 April 2022

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 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

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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

characterization techniques. Using Scanning electron microscopy, Energy dispersive spectroscopy

and X-ray diffractometry we have identified the grain morphology, chemical composition, and

crystal structure of the powder.

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 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

for high temperature applications.

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

structure of the powder sample.

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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

help us identify the morphology and microstructure of the materials.

Figure 1 SEM micrographs of MoSi2 powder from low to high magnification

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

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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

the morphology of the powder sample under investigation.

Figure 2 Surface morphology of MoSi2 powder

Energy Dispersion Spectroscopy:

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

material under inquiry.

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

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phases in the microstructure. While the second image shows compositions of different elements in

A, B, C, and D phases which are present in the microstructure.

Figure 3 BSE image of MoSi2 powder

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

composition of MoSi2 is much more than Mo5Si3.[1]

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 Figure 4 EDS spectrum of MoSi2 powder

The ratio of MoSi2/Mo5Si3 in phases A, B, C, and D is given in the table below.

Phases MoSi2/Mo5Si3

A Single phase region, 100% MoSi2

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

i.e., B, C, and D there is some amount of Mo5Si3 present.

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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.

Melting temperature of MoSi2 is 2020°C and at the temperature of 1900°C it undergoes a

polymorphic transformation from low temperature tetragonal form (α-MoSi2) to high-temperature

hexagonal form (β-MoSi2) [2]. MoSi2 is most interesting industrially for its excellent oxidation

and corrosion resistant properties at high temperatures.

Figure 5 X-ray diffraction pattern of MoSi2 and Mo5Si3 phases (λ-Cu Kα) after Si reaction with Mo at 1530◦ C, 3 min

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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

whole powder pattern fitting (WPPF) as an alternative to quantify them. [3]

Figure 6 Quantitative analysis of MoSi2 and Mo5Si3

Indexing of the Peaks:

Figure 7 XRD pattern of MoSi2

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Indexed Pattern of MoSi2:

2θ θ d-spacing(a0) 𝟏 𝟏/𝐝𝟐 𝟏/𝐝𝟐 h k l

𝐝𝟐 𝟎. 𝟎𝟔𝟕 𝟎. 𝟏𝟏𝟑
(a-2)

23 11.5 3.86 0.067 1.00 0.592 0 0 1

30 15 2.97 0.113 1.68 1.00 1 0 0

39 19.5 2.30 0.189 2.82 1.67 1 0 1

45 22.5 2.01 0.247 3.68 2.08 1 1 0

47 23.5 1.93 0.268 4 2.37 1 1 1

57 28.5 1.61 0.385 5.74 3.40 1 0 2

63 31.5 1.47 0.462 6.89 4.08 2 0 0

66 33 1.41 0.503 7.50 4.45 2 0 1

73 36.5 1.29 0.600 8.99 5.03 2 1 0

76 38 1.25 0.640 9.55 5.66 2 1 1

77 38.5 1.23 0.661 9.86 5.84 0 0 3

86 43 1.12 0.797 11.89 7.05 2 0 2

The (h, k, l) values comes from the indexing of the pattern shows the Tetragonal crystal

structure of MoSi2.

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Unit Cell of MoSi2:

Figure 8 Tetragonal unit cell structure of MoSi2 (a=0.3205, c=0.7845 nm)

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

1900°C MoSi2 transforms from a tetragonal (C 1 1 b type, a = 0.3202, c = 0.7851 nm) to a

hexagonal (C 4 0 type) crystal structure.

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

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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

the powder in the applications where these properties are beneficial.

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.

[2] (N.d.). Researchgate.Net. Retrieved April 17, 2022,

fromhttps://www.researchgate.net/figure/X-ray-diffraction-pattern-of-MoSi2-and-
Mo5Si3-phases-CuK-after-Si-reaction-with-Mo-at_fig1_288815268

[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

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