Fabrication of ceramic matrix composite by using microwave energy

Harpreet Singh et al., International Journal of Advanced Research in Innovative Discoveries in Engineering and Applications[IJARIDEA]
Vol.1, Issue 2,27 December 2016, pg. 1-8
1
© 2016, IJARIDEA All Rights Reserved
Fabrication of ceramic matrix composite by
using microwave energy
Harpreet Singh1
, Mandeep Singh2
, Ranjit Singh3
, Shavinder Singh4
1,2,3,4
Lovely Professional University, India.
Abstract— Nowadays, ceramic matrix composites are being extensively used for industries and household
purposes. However, these ceramic composites materials are substantially resistant to biodegradation. In this
experimental study the specimen of silicon carbide with varying percentage of titanium carbide (TiC) has
been fabricated by using microwave sintering. Different samples having TiC 5%, 10%, 15% (wt%) were
prepared by die pressing. Then sample were heated in microwave furnace at different range of temperatures
i.e. 1150°C, 1250°C and 1350°. It was found that with increase in the weight percentage (wt %) of TiC, the
porosity was maximum in 1150°C and minimum porosity achieved maximum temperature 1350°C. The
maximum hardness was achieved in 1350°C when 15 wt % of TiC. Density was also increased with respect to
the increase in temperature and TiC wt %.
Keywords— Ceramic Matrix Composite; Hardness; Microwave Heating; SiC; TiC.
I. INTRODUCTION
Ceramic matrix composite (CMC's) were developed to overcome essential brittleness and
many reliability of massive and uniform ceramic, with a view to introduce ceramic in
structural part used in various environments, such as rocket and jet engines, gas turbines for
power plants, heat shield for space vehicles etc[3,8]. It is generally admitted that the use of
CMS's in advanced engine can be operated and eventually the elimination of the cooling
fluids, both resulting in an increase of yield. There is a wide spectrum of CMS's depending
on the chemical composition of the matrix and reinforcement [12]. Non-oxide CMS's are by
far those which have been the most studied [11].
Among the various non-oxide ceramics that found commercial applications, silicon carbide
(SiC) is the leader. Silicon Carbide is the main concoction compound of carbon and silicon.
Attractive properties, such as good specific strength and Young’s modulus as a function of
temperature, the specific stiffness, corrosion and erosion resistance made SiC an attractive
alternative to the hard metal compositions [7]. SiC has turned a special attention as advanced
ceramic material recently since it offers superior properties such as high hardness, low bulk
density, high oxidation resistance, thermal conductivity and thermal shock resistance [9].
Furthermore, it is an important ceramic used in structural applications, such as automotive
engines, cutting tools, heat exchange and mechanical seals [2,10]. Additionally, it is used in
bulk form as refractory products, as electric heating elements and resistors, as igniters for gas
appliances, as ceramic burners, as mechanical seal faces, as radiation sensors, as low-weight
high-strength mirrors, as high power and high temperature semiconductor devices, as
radiation resistant semiconductors and as light-weight armors [2, 13].
Silicon Carbide is the base material another material is Titanium Carbide Titanium carbide
is a to a great degree hard obstinate earthenware material, like tungsten carbide. This
experiment using two additives yttrium oxide and aluminum oxide both have great heat
conductivity.PVA is a colorless, water-soluble synthetic resin employed principally in the
treating of powder. For making pellets in laboratory scale processing normally we make 2-
5 % PVA solution in distilled water (2.5gm PVA in 98 ml water). Christo Ananth et al.[4]
discussed about E-plane and H-plane patterns which forms the basis of Microwave
Engineering principles.

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II. EXPERIMENTAL PROCEDURE
The development of composite material is based on formulation in the binary SiC-TiC
system with small amount of sintering aids. As a major raw material black and white high
purity SiC powder of different grades (CDH Central drug (P) house, size grain size 68 micron
meter) are used. TiC powder used in Titanium (NANOSHEL Chandigarh, size 25 micron
meter). Aluminum oxide is used manufactured by NICE chemicals (P) ltd, grain size 90
micron meter. Yttrium oxide are used LOBA Chemie, size 95 micron meter, chemical
formula Y2O3 and PVA are used LOBA Chemie, chemical formula: (C2H4O)n.
A. Sample Preparation
Three different powder batches having different nominal ceramic composites were
prepared as follows: A (5% TiC- 89% SiC- 3.6% Al2O3- 2.4% Y2O3), B (10% TiC- 84% SiC-
3.6% Al2O3- 2.4% Y2O3), C (15% TiC- 79% SiC- 3.6% Al2O3- 2.4% Y2O3).
The constituent material we had used is SiC, TiC, Al2O3 and Y2O3 with specified weight
percentage of the total weight of the specimen. After that the ball mill was used to mix the
powder at rotational speed of 65 RPM for 5 hours. The constituent particles are in powder
form which was moisturized by a solution of PVA 2.5% in 98ml distilled water for making
green specimen.
Pellets were made by dry pressing in a hydraulic pressing at a load of 3.5 MPa with a 25 %
pump speed and dwell time of 90 seconds. A high carbon, steel die (10 mm diameter) was
used. The pellet thickness was 5 mm. Green compaction performed in LALCO Industries
Manufacturers of Diesel Engine Spare Guru Teg Bahadur Nagar, Phagwara 144401.
Specimen after compaction and drying process has been shown in Fig.1 and 2 respectively.
Fig.1 Green specimen of the SiC and TiC (W%- 10%).

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Fig.2 After removing in muffle furnace for reduce the moisture of green specimen, the temperature of the muffle furnace was 500°C
Sintering of the pellets was sintered in a microwave vacuum furnace (Omicron Scientific
Equipment Company) with heating element at 11500
C, 12500
C and 13500
C. At each sintering
temperature, the holding times for different batches were 10 minute. An intermediate soaking
period of one hour at 5000
C was provided for binder removal by muffle furnace. Sintering
performed in Omicron Scientific Equipment’s Company 309, Vardhman Sudarshan Plaza,
Plot No. 4, M.L.U. Sector 5,Dwarka, New Delhi 110075. Specimen after microwave sintering
at 13500
C has been shown Fig.3.After sintering the specimen was subjected to different test
to find out the mechanical properties of the ceramic composite.
Fig.3 Microwave sintering the green specimen at 1350°C
B. Density
To measure the density, firstly we had find the mass and the volume by using the weighing
machine and Vernier caliper and micrometer to measure the diameter and length of the
cylinder respectively. It is then assessed from the recipe given underneath. [4-6]
Density (g/cm3
) = (1)
Unit of the density = g/cm3
C. Porosity
Porosity begins from the voids, which are made inside of the mass. These pores are of two
sorts; open and shut pores. The open or also called obvious porosity measures the portion of
void volume to the material volume. The open pores are normally interconnected so they give
sections through which gasses can pass. [1]
The accompanying technique was utilized as a part of deciding the porosity. The specimens
were kept in the broiler at 1100
C for 3h to get steady weight W1. The specimens was then
suspended in refined water and bubbled on a hot plate for 30 minutes. In the wake of
bubbling while still in boiling hot water, the water was dislodged with cool water, the weight
W2 was measured on an advanced offset depended on the tripod stand. The test example was
expelled from the water and additional water wiped off from the surface by softly blotching
the specimen with wet towel and the weight W3 of the absorbed specimen suspended air was
measured. The obvious porosity of the example was resolved from the relationship. [5]
Pa= Apparent porosity
W1= Weight in air
W2= Weight of the sample
W3= Weight of the cold water
Specimen

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Pa= (W3 --W1)/ (W3--W2)
D. Vicker Hardness Test
It is the standard technique for measuring the hardness of metals, especially those with
greatly hard surfaces: the surface is subjected to a standard weight for a standard period of
time by method for a pyramid-formed precious stone.
The Vickers hardness test system comprises of indenting the test material with a precious
stone indenter, as a right pyramid with a square base and a point of 136 degrees between
inverse confronts subjected to a heap of 1 to 100 kgf. The full load is regularly petitioned 10
to 15 seconds. The two diagonals of the space left in the surface of the material after
evacuation of the heap are measured utilizing a magnifying instrument and their normal
computed. The range of the slanting surface of the space is ascertained. The Vickers hardness
is the remainder acquired by partitioning the kgf stack by the square mm range of space. [5]
HV= 1.854 (2)
F= load in kgf
d= Arithmetic mean of the two diagonal, diameter and length in mm.
HV= Vicker Hardness.
E. Microstructural Examination
The selected sintered samples were viewed in optical microscopic. The images were taken
using optical microscope using image analysis software. Magnification of 500X was used
while procuring the image. The sample were placed on a slide and then viewed through the
monitor screen.
III. RESULT AND DISCUSSION
The study of mechanical properties of the ceramic composite are mainly depend on density,
Apparent Porosity, Vickers Hardness and microstructure. The microstructure developed for
various TiC additions.
A. Density
From the density result it can be seen that the presence of SiC material has some effect on
the density of the CMCs. Density of SiC powder were measured to vary 1.66 to 1.93 g/cc and
those for the TiC powder were around 4.93 g/cc. Results for the density of the SiC- TiC with
varying percentage (5%, 10%, 15%) and temperature is shown in the Fig.4

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Fig.4 Density for SiC- TiC composite with varying wt % of TiC at different temperature
B. Apparent Porosity
Porous ceramics have turn out to be progressively vital in industry as of late because of
their various applications and uses including distinctive materials like metals, pottery,
polymers, composites, semiconductors and biomaterials [14]. The porosity decreased as the
weight fraction of TiC % particles and temperature increased.
Fig.5 Apparent Porosity for SiC- TiC composite with varying wt % of TiC at different temperature
C. Vicker Hardness
Measure of hardness, is to watch the investigated material's ability to restrict plastic
deformity from a standard source. The Vickers test can be used for all metals and has one of
the amplest scales among hardness tests.
The Vicker hardness value increased as the weight fraction of the TiC % particles and
temperature increased. Because the aluminum oxide and yttrium oxide react with the help of
PVA when increase the temperature. TiC particles are occupy the particle gap because
particles size is very small compare to the SiC. Fig.6 depicts the value for microhardness.

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Fig.6 Micro hardness for SiC- TiC composite with varying wt % of TiC at different temperature
D. Microstructure
Fig.7 Shows the microstructure of SiC reinforced with TiC. The structure revels the brittle
ceramic phase which is dark in color.
Fig.7 Microstructure was observed at 1150°C
Micrograph the microstructure of the reinforced tin tailing reveals that there are some
discontinuous and a reasonably uniform distribution of TiC 15% particles. In Fig.8, Bright
particles are SiC and dark particles are TiC.

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Fig.8 Microstructure was observed at 1350°C
IV.CONCLUSION
Therefore we conclude from the result that the variation in the density, porosity and
hardness occurs with the change in the sintering temperature and percentage of TiC. From the
graph we observe that the increase in the sintering temperature the hardness and density of
the material is increasing significantly similar phenomenon we have observed from the
literature survey. The increase in the sintering temperature possibly increase the material
atomic kinetics which helps in homogenous distribution of the added material, this may be
the reason for increasing the density and hardness of the samples. Secondly, we have seen the
same observation with the increase in the TiC percentage, The increase in the percentage of
the TiC decreases the intermolecular voids decreases that we see from the micrographs and
even observed from the literature survey that the increase in the percentage of the TiC the
Density increases, TiC is a very small size particle compared to SiC so it occupies the
intermolecular space in between the SiC molecules. The porosity and density have inverse
relation like we have seen in the literature review and observed from the micrographs that the
intermolecular voids are decreasing that simply signifies the porosity of the material
decreasing with the addition of the TiC and increase in the sintering temperature.
REFERENCES
[1] W, D. Callister, Jr “Materials Science and Engineering”. 1997, 511-531.
[2] R. Hamminger, Carbon Inclusions in Sintered silicon Carbide, Journal of the American Ceramic Society
72/9 (1990) 1741-1744.
[3] K.U. Kainer, “Metal Matrix Composites Custom-Made Materials for Automotive and Aerospace
Engineering”, Wiley-VchVerlag GmbH & Co. KGaA, Weinheim, 2006.
[4] Christo Ananth, S.Esakki Rajavel, S.Allwin Devaraj, M.Suresh Chinnathampy. "RF and Microwave
Engineering (Microwave Engineering)." (2014): 300.
[5] V.S Aigbodion& S.B .Hassan “Effects of silicon carbide reinforcement on microstructureand properties of
cast Al-Si-Fe/Sic particulate composites”, Journal of Materials Science and Engineering A, 2007, 447,
355-360
[6] I.A. Ogucha “Characterization of Aluminum Alloy 2618 and its Composites ContainingAlumina
Particles,” Ph.D Dissertation Department of Mechanical Engineering, University ofSaskatchewan,
Saskatoon, 1997, 1-2000.
[7] J. Marchi, J.C. Bressiani, A.H.A. Bressiani, “Densification Studies of Silicon Carbide-Based Ceramics
with Yttria, Silica and Alumina as Sintering Additives”, Materials Research 4 (2001) 231-236.
[8] R. Naslain, Université Bordeaux 1, 33600, Pessac, France.

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[9] S. Prochazka, Hot Pressed Silicon Carbide, US Patent 3853566, 1974.
[10] W. van Rijswijk, A.R. Raffray, “Effects of Carbon as a Sintering Aid in Silicon Carbide”, Journal of the
American Ceramic Society 73/1 (1990) 148-149.
[11] J.B. Wachtman, Mechanical Properties of Ceramics, John Wiley and Sons Inc., New York, 1996.
[12] A.W. Weimer, “Carbide, Nitride and Boride MaterialsSynthesis and Processing”, Springer, New York,
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[13] R.W. Williams, B.N. Juterbock, C.R. Peters, T.J. Whalen, “Forming and sintering behavior of B- and C-
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[14] Muhammad SyamilJunid, “The Fabrication of Porous Ceramic,” Proceedings of 2008 student conference
on research and development, Technical University of Malaysia, May 2008.
[15] S. Abdul Gaffar, O. Anwar Beg, E. Keshava Reddy, V. Ramachandra Prasad, "Mixed Convection
Magnetohydrodynamic Boundary Flow And Thermal Convectionof Non-Newtonian Tangenthyperbolic
Fluid From Non-Iosthermal Wedgewith Biot Number Effects.", International Journal of Advanced
Research in Innovative Discoveries in Engineering and Applications[IJARIDEA], Volume 1,Issue
1,October 2016,pp:7-11

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