Fabrication and Microstructure of Micro

and Nano Silicon Carbide Reinforced

Copper Metal Matrix Composites/
Nanocomposites

Amar Mahato & Subrata Mondal

Silicon

ISSN 1876-990X
Volume 13
Number 4

Silicon (2021) 13:1097-1105

DOI 10.1007/s12633-020-00491-5

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 Author's personal copy
Silicon (2021) 13:1097–1105
https://doi.org/10.1007/s12633-020-00491-5

ORIGINAL PAPER

Fabrication and Microstructure of Micro and Nano Silicon Carbide

Reinforced Copper Metal Matrix Composites/Nanocomposites
Amar Mahato 1 & Subrata Mondal 1

Received: 12 November 2019 / Accepted: 22 April 2020 / Published online: 4 June 2020
# Springer Nature B.V. 2020

Abstract
This study investigates the influence of micro and nano silicon carbide on properties of copper matrix composites/
nanocomposites containing up to 4 wt% of reinforcement concentration. It was observed that an increase of SiC (both micro
and nano sized) content resulted in a higher hardness, compressive strength and better wear properties. However, nano SiC
reinforced composite materials have better hardness, compressive strength and wear properties as compared with micro sized SiC
reinforced composites. Grain refinement of composite/nanocomposite materials as compared with pure copper materials were
observed from the metallurgical microscopic images. Further, scanning electron microscopic images revealed uniform
dispersion/distribution of reinforcing materials in the copper matrix, and good bond formation between component materials.
As the micro/nano sized SiC reinforcement in the copper matrix decreased the density of resultant composite/nanocomposite
materials, therefore, nano sized SiC reinforcement will be helpful to fabricate light weight copper matrix nanocomposite
materials for various industrial applications.

Keywords Compressive strength . Interfacial bonding . Metal matrix composite . Morphology . Silicon carbide

1 Introduction ceramic matrix [3]. In the metal matrix composite, metal or

Composite materials are prepared by the combination of two
or more materials, where individual component retain their
identity, while, bonded together by physical and/or chemical
bonding. The major portion of material in the resultant com-
posite is termed as matrix phase or continuous phase, while,
the minor phase of the material is termed as the reinforcing
phase or dispersed phase. Generally, reinforcing phase is
harder than the matrix phase of composite materials. There
are several advantages of composite materials as compared
with pure matrix material such as high specific strength, better
hardness, and improvement of other functional properties
which depends on the type of reinforcing materials.
Depending on the type of matrix phase, composite can be
categorized by polymer matrix [1], metal matrix [2] and
* Subrata Mondal
subratamondal@yahoo.com
1
Department of Mechanical Engineering, National Institute of
Technical Teachers’ Teacher Training and Research (NITTTR),
Kolkata, FC Block, Sector III, Salt Lake City, Kolkata, West
Bengal 700106, India
alloy is the matrix phase or continuous phase, and reinforce-
ment can be various type of inorganic, carbon based or ceram-
ic based materials [4–6]. Metal is the primary component for
many structural, electrical and thermal applications, therefore,
significant efforts have been made in order to enhance their
properties by using suitable reinforcements like aluminum
oxide, carbon, micro and nano silicon carbide etc. [7–10].
Cu, Mg and Al or their alloys have been widely used for the
production of metal matrix composites (MMC) reinforced by
nano and micro particles such as carbides, nitrides, oxides
[11–14]. Recently, there are significant research interests on
copper metal matrix composites using various types of micro/
nano reinforcements. In various engineering applications cop-
per alloy makes most preferable material due to relatively low
cost, increased strength to weight ratio, good thermal/
electrical conductivity and other interesting characteristics.
Weak properties of copper can be enhanced by the reinforce-
ment of specific reinforcing materials in order to enhance
properties of resultant composite materials and to make it
suitable to be used in various structural applications [15–19].
Various types of ceramic and other inorganic particles/fi-
bers/flakes can be reinforced into the copper matrix to manu-
facture metal matrix composites. Common reinforcement
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materials for the metal matrix composites includes alumina
[10, 17], boron carbide [20], silicon carbide [21, 22], various
carbon materials viz. graphene [23, 24], carbon nanotube [23,
25], carbon nanofiber [26] etc. Silicon carbide both micro and
nano size particulates can be considered as very good rein-
forcing materials in various metal matrix composites/
nanocomposites for the enhancement of various functional
properties. Chmielewski et al. reported tungsten coated micro
SiC particle reinforced copper matrix composites fabricated
by using hot pressing (HP) and spark plasma sintering (SPS)
technique. Spark plasma sintering process produced compos-
ite with higher interfacial strength than the hot pressing pro-
cess [27]. Ayyappadas et al. compared properties of micro SiC
reinforced copper matrix composites produced by using con-
ventional sintering and microwave assisted sintering.
Microwave assisted sintering process provide better densifica-
tion of composites as compared with conventional sintering
method. Further, microwave sintered composite showed bet-
ter mechanical, electrical and frictional properties as compared
with conventional sintered samples [15]. Fatoba et al. reported
various micro sized SiC reinforced composites produced by
using liquid metallurgy method. Electrical and thermal con-
ductivity of composite materials were reported with respect to
the particle size of SiC [22].
Metal matrix composites/nanocomposites can be fabricated
by using three basic process viz. solid state process, liquid
state process and solid-liquid mixed process. Stir casting,
squeeze casting and spray casting are some of the liquid state
process, while, powder technology and friction stir casting are
solid state process for MMC fabrication, and compo casting
and semi solid forming are categorized as liquid-solid mixed
process for the fabrication of MMC [28–32]. Key factors
which influences the properties of surface composites pro-
duced by friction stir processing are process parameters (rota-
tional speed, traverse speed and tilt angle), tool geometry, tool
dimension and reinforcement strategies [33]. One of the major
disadvantages of friction stir process is reinforcing particle
agglomeration due to the inadequate heat generation and
asymmetric nature of material flow during friction stir passes
[34, 35]. Among the solid state process viz. friction stir pro-
cess and powder metallurgy methods, powder metallurgy
method has several advantages such as simple process (pro-
cess steps: mixing-compaction-sintering), reduction of scraps,
high production rate, elimination of machining, production of
complex shapes etc. [36, 37]. There are several research pa-
pers reported the fabrication of SiC reinforced copper matrix
composites. However, in our knowledge a comparison of mi-
cro and nano SiC reinforced copper matrix composites is rare-
ly reported. This study presents fabrication and characteriza-
tion of copper matrix composites and nanocomposites by
using SiC micro and SiC nano fillers, respectively. Powder
metallurgy method was used for the fabrication of composite/
nanocomposite materials. Properties of micro and
Silicon (2021) 13:1097–1105
nanocomposites are compared, and correlated with micro-
structure and morphology of specimens.
2 Experimental
2.1 Materials
In this research, copper has been selected as the matrix phase.
Two types of silicon carbide viz. micro size and nano size
were used as reinforcement phase for the fabrication of copper
matrix composite/nanocomposite. Copper powder (purity
99.5%) and micro sized silicon carbide (99.7%) were pur-
chased Loba Chime Private Limited, Mumbai, while, nano
size silicon carbide (purity 98%) was procured from S. R. L.
Private Limited, Mumbai. Particle size of micro SiC and nano
SiC were 20 μm and 50 nm, respectively.
2.2 Fabrication of Composites/Nanocomposites
Powder metallurgy method was employed for the fabrication
of metal matrix composites and nanocomposites. The basic
steps for fabricating SiC reinforced copper matrix
composites/nanocomposites were mixing silicon carbide with
metal powder, followed by consolidation by compaction and
sintering. The ball milling type mixing method was adopted
for mixing of pure metal and reinforcement powder by using a
Lathe (Panther, Gujarat Lathe Mfg. Co. Pvt. Ltd., India).
Compaction step was performed by a universal testing ma-
chine. Specially designed die was used to prevent the defor-
mation during compaction under high pressure. Powder mix-
ture was compacted at constant compaction pressures
(636 MPa) to obtain the cylindrical shape samples. In powder
metallurgy, sintering is an important method to increase the
adhesion between component particles. As the melting point
temperature of copper is around 1060 °C therefore, pure
compacted metal and metal matrix composites/
nanocomposites samples were sintered at temperature below
the melting point temperature of matrix materials in order to
keep the cylindrical shape of the samples. Further, sintering
process was carried out in vacuum (an oxygen free environ-
ment), in order to prevent the oxidation of specimens.
2.3 Characterizations of Composites/Nanocomposites
Densities of specimens were measured by taking weight and
dimension of specimens (ρ = m/V). Dimension of specimens
was measured by Vernier caliper and weight was measured by
digital weighing balance. Density measured before sintering is
labeled as green density, while, after sintering is labeled as
sintered density. Specimens with approximate 30 mm length
and 10 mm diameter in cylindrical shape were prepared for
measurement of hardness and compressive strength. Sintered
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Silicon (2021) 13:1097–1105
specimens were polished carefully prior to the measurements.
Hardness of specimens were measured by using Rockwell
hardness tester (Model No TRS, Fine Testing Machines Pvt.
Ltd., India) with a constant load of 100 Kgf with 1/16 in. steel
ball indenter. Compressive strength of the samples was mea-
sured by using universal testing machine (UTM) (Model No
SOM205, Neelam Engineering Company, India). Dimeter
and length of the cylindrical specimens used for compressive
test were around 10 mm and 30 mm, respectively. During the
compressive test, upper movable jaw compresses the material
and deforms the material until it fails. Figure 1 shows the
image of copper cylindrical specimen before and after com-
pressive test. Final reading of specimen can be obtained from
the display of the machine. All reported results are average of
three readings. Friction and wear rate of specimens are char-
acterized by using friction and wear tester (TR 201, DUCOM
Triboinovators). Weight loss of the material is related to wear
rate. From the contact surface of the cylindrical specimen (the
pin of 10 mm diameter) which was in contact with the rotating
disc, wear rate was measured by removing the material. Wear
rate was calculated by using the following relationship:
Specific wear rate, Wsp = wear volume/(normal load x
total sliding distance) mm3/N-m.
We know that, sliding speed = πDN/1000 m/min = πDN/
(1000 × 60) m/s.
where, D = Track diameter (in terms of mm), N = rpm, D in
all measurement was fixed at 70 mm.
Microstructure of specimens were characterized by using
metallurgical (Leica DM2700M). Prior to microstructure ob-
servation, specimens were polished by using emery paper and
subsequently etched with acid solution (distilled water-92 ml,
nitric acid-6 ml, hydrofluoric acid- 2 ml). Samples were ob-
served under optical microscope with maximum 50X magni-
fication. Scanning electron microscope (SEM) was employed
to study the surface morphology and dispersion/distribution of
reinforcements (micro SiC and nano-SiC) particles in copper
matrix. SEM used for this study is manufactured by ZEISS
Fig. 1 Image of cylindrical specimen before and after compressive
testing
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EVO 18. All samples were coated with platinum prior to the
SEM observation. Microstructure of specimens was observed
at various magnifications from 1000X to 50,000X.
3 Results and Discussion
3.1 Properties of Micro/Nanocomposites
Green densities and sintered densities of samples were inves-
tigated after compaction and sintering (Table 1), respectively.
Density of composite depends on particle size, shape, fraction
of components, nature of reinforcements, and packing of mol-
ecules [38]. Experimental results revealed that the sinter den-
sity is more than that of the green density because of particles
packing, more compact structure formation. Sintered density
of samples decreased with the increase in SiC as compared
with pure copper sample due to the lower density of SiC
(~3.21 g/cc) as compared with pure copper (~8.96 g/cc).
However, green and sintered density of nano SiC reinforced
composites is slightly higher than that of the micro SiC rein-
forced composites due to the better packing of particles.
Lower density of micro SiC reinforced specimen is due to
coarse nature of particles, hence, poor packing of particles as
compared with nano SiC [38]. 4 wt% of micro SiC imparts
lower densification of compacted material. This is probably
due to the fact that higher concentration of hard SiC micro
particles prevent copper to plastically deform during the com-
paction process. Therefore, with the addition of higher con-
centration of micro SiC will result in lower densification of
composite material [15]. Figure 2 shows that hardness in HRB
of composite/nanocomposites is higher than that of the pure
Cu due to the hard nature of SiC due to the covalent and ionic
bond in the ceramic particles [39]. Hard reinforcing particles
holds soft matrix phase, which makes composite strong in
nature [38]. Increase hardness of the composite or nanocom-
posite materials is due to the particle strengthening and Orwan
strengthening due the presence of bonded SiC particles in the
copper matrix [40]. Further, grain refinement can also en-
hances the hardness of composite and nanocomposite mate-
rials [41]. Hard SiC particles are excellent barrier for disloca-
tion of soft copper matrix. With an increasing SiC concentra-
tion in the copper matrix, strongly hinder the plastic flow as a
result of higher hardness value [15]. Experimental result re-
vealed that hardness of the nano-particles silicon carbide rein-
forced composites is higher than micro silicon carbide com-
posites due to more compact structure formation and better
interfacial bond strength between particles (see SEM result).
Further, nano sized SiC produces higher Orowan strengthen-
ing effect due to the smaller particle size and lower inter par-
ticle spacing as compared with micro sized SiC [42].
Compressive strength of pure compacted and sintered cop-
per sample is 281.2 MPa, and with the introduction of 1 w/w%
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1100 Silicon (2021) 13:1097–1105

Table 1 Properties of micro/nano

sized silicon carbide reinforced Properties of micro/nano Reinforcement conc. (w/w%)
composites/nanocomposites composites
Micro sized SiC Nano sized SiC

0 1 2 4 0 1 2 4

Green density (g/cc) 7.41 6.80 6.75 7.10 7.41 7.38 7.28 6.81
Sintered density (g/cc) 7.55 6.98 6.96 6.64 7.55 7.55 7.32 6.98
Compressive strength 281.2 310.1 405.1 695.2 281.2 336.6 459.1 713.7
(MPa)

micro silicon carbide in the composite matrix, compressive
strength is increased to 310.1 MPa. Further, with 2 w/w %
and 4 w/w% micro silicon carbide, the compressive strength
increases to 405.1 MPa and 695.2 MPa, respectively.
Experimental result revealed that compressive strength in-
creases with increasing micro silicon carbide concentration
in the matrix due hard nature of SiC, and strong bond forma-
tion between SiC and Cu matrix [43]. Compressive strength of
1 w/w% nano-particles SiC reinforced composite has been
increased from 281.2 MPa to 336.6 MPa. With further in-
crease of nano SiC such as 2 w/w% and 4 w’w% nano-
particles in the composite samples, the compressive
strength increased to 459.1 MPa and 713.7 MPa, respec-
tively. From experimental results, it was found out that
compressive strength increases with increasing nano-
particles SiC concentration in matrix due to more compact
structure formation (because of better packing of mole-
cules) after sintering, which increases cohesive strength
between molecules. Further, presence of hard reinforce-
ment in the soft copper matrix restrict the dislocation mo-
tion and plastic flow of matrix material as the ceramic
reinforcement particles are interlock between the metal
matrix grains which in turn increases the compressive
strength of material with increasing reinforcement concen-
tration in the matrix [44]. Higher compressive strength of
nano SiC reinforced nanocomposites as compared with
same concentration of micro SiC is due to the higher hard-
ness and more compact structure of the material.
Wear resistance of specimens was tested by using wear and
friction monitoring machine. Wear in μm of composite/
nanocomposites specimens at 50 N load and various sliding
speed 550 rpm, 650 rpm, 750 rpm is shown in Fig. 3. Wear
resistance of SiC reinforced composite/nanocomposite is bet-
ter as compared with pure Cu possibly due to the increasing
hardness of specimen [39]. Wear rate of the composites and
nanocomposite materials decreases with increasing reinforce-
ment concentration in the copper matrix due to the hard SiC
particles which took up the load [40]. Wear test result revealed
that wear increases with increasing speed due to the plastic
deformation of the particles from the composite, because of
the higher friction produced at higher rpm [39, 44]. Wear
decreases with increasing reinforcement concentration in the
specimens due to the formation of lubricating film on the worn
surface [38]. Specific wear rate of nanocomposite samples is
shown in Fig. 4. Nano SiC particle plays prominent role for
the improvement of tribological property of nanocomposites.
Pure Cu shows higher specific wear due to the identical nature
of molecules which increases plastic flow of materials, and
presence of reinforcing material reduces plastic flow.
3.2 Microstructure and Morphology of
Composite/Nanocomposite Specimens
Figure 5 shows the metallurgical microscopic images of pure
copper and composite/nanocomposite samples. Micrograph
revealed uniform homogeneous structure of pure copper

Fig. 2 Variation hardness 90 Micro SiC

property of composite/ Hardness (HRB)
nanocomposite with 85
Hardness (HRB)

reinforcement concentration 80 Nano SiC Hardness

(HRB)
75
70
65
60
55
50
0 1 2 3 4 5
SiC (wt%)
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Silicon (2021) 13:1097–1105 1101

Fig. 3 Wear rate of specimens at Pure Cu

50 N load with various speed: (a) 60
microcomposite samples and (b) 55 Micro SiC 1%
nanocomposite samples
50 Micro SiC 2%

Wear (µm)
45 Micro SiC 4%
40
35
30
25
20
500 600 700 800
Speed (rpm)

(a)

60 Pure Cu
55 Nano SiC 1%
50 Nano SiC 2%
Wear (µm)

45
Nano SiC 4%
40
35
30
25
20
500 600 700 800
Speed (rpm)

(b)

sample and presence of single phase (Fig. 5a). Porosity in few
places can be observed due to improper compaction which
introduces air in the specimen, and this entrapped air would
remove during sintering process and formed porosity.
Presence of copper and SiC particles is observed in the micro-
graph of microcomposite sample (Fig. 5b) with 4 wt% of
micro SiC. The matrix phase indicates the improper
distribution of reinforcement phase possibly due to the ag-
glomeration in few places. Micrograph of 4 wt% nano SiC
reinforced nanocomposite specimen (Fig. 5c) revealed pres-
ence of copper in light portion whereas dark portion represents
agglomeration of nano silicon carbide in few locations.
Optical micrographs did not show any intermediate phase be-
tween copper and silicon carbide interface which indicates

Fig. 4 Specific wear rate of 0.0006 550 rpm

specific wear rate in (mm3/N-m)

nanocomposite samples at load

with various speed 0.0005 650 rpm

0.0004 750 rpm

0.0003

0.0002

0.0001

0
0 1 2 3 4 5

Nano SiC (wt%)

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1102 Silicon (2021) 13:1097–1105

nano particles can delay the crystal growth of grains during

sintering process [45]. Microscopic images revealed that nano
SiC reinforcement induces better grain refinement of Cu par-
ticles as compared with the micro SiC reinforcement.
Properties of composites/nanocomposites depends on mi-
crostructure and morphology of specimen. Properties of spec-
imens are correlated with the micro structure of samples. The
functional and mechanical properties of reinforce composites
depends upon the distribution and dispersion of micro and
nano-particles in the copper matrix, interfacial bond formation
between reinforcement phase and matrix phase. Figure 6a and

Fig. 5 Metallurgical microscopic images of specimens: (a) pure copper;

(b) microcomposite with 4 w/w% SiC and (c) nanocomposite with 4
w/w% SiC

that no reaction has been takes place during sintering process.

Reinforcing micro/nano SiC in the Cu matrix improves the
grain refinement. Microscopic images revealed that grain
around SiC are much finer than the grains around SiC free
matrix. Therefore, SiC particles can induce recrystallization
of copper matrix by accelerating particle nucleation between Fig. 6 Scanning electron micrographs of: (a) pure copper and (b)
reinforcement particle and matrix phase. Further, SiC micro/ microcomposite with 2 w/w% SiC
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Silicon (2021) 13:1097–1105
Fig. 7 Scanning electron microscopic images of nanocomposite
specimens: (a) 1 w/w% nano SiC; (b) 2 w/w% nano SiC and (c) 4
w/w% nano SiC
1103
Fig. 6b shows pure Cu and 2 w/w% micro SiC reinforced
composite, respectively. Surface morphology revealed pres-
ence of pores in the composite and pure Cu sample due to the
presence of bigger particles. Presence of pore can influences
density, tribological and mechanical properties of the mate-
rials. Changes of microstructure of microcomposite can be
observed as compared with pure Cu, therefore, micro SiC
altered the copper matrix [12]. SEM micrograph of micro
SiC composite revealed uniform dispersion of micro SiC,
and no visible gap between Cu matrix and reinforcement
phase, hence, component particles are adhered with each other
after sintering. Apart from Cu-SiC interphase, no other phase
were observed in the SEM micrographs [15] and this con-
firmed the non-formation of any intermediate product during
the sintering process. Micrographs of nanocomposite samples
revealed no significant agglomeration of reinforcement phase
with 1 and 2 w/w% of nano SiC in the copper matrix phase
(Fig. 7a and b) which confirmed good dispersion of nano SiC
in the copper matrix, and no visible gaps between matrix
phase and nano reinforcement phase, hence, perfect bond for-
mation between various phases. Microstructure of nanocom-
posite sample with 4 w/w% of nano SiC revealed agglomera-
tion of nanoreinforcing phase in few locations, however, ex-
cellent bond formation between component particles and po-
rosity in few places. SEM micrographs of 4 w/w% nano-
particles silicon reinforced copper matrix nanocomposite
(Fig 7c) revealed presence of more nano SiC on the surface
which confirms good distribution of nano SiC.
4 Conclusions
In this work, SiC reinforced copper based metal matrix
composites/nanocomposites were successfully fabricated by
using powder metallurgy technique. The effects of micro sized
SiC and nano sized SiC on density, Rockwell hardness, com-
pressive strength and wear properties have been examined.
Density of composite/nanocomposite materials slightly de-
creased irrespective of size and concentration of SiC.
Compressive strength and hardness value have been increased
with increasing reinforcement concentration in the metal ma-
trix. Maximum compressive strength was measured as
713.7 MPa with 4 wt% of nano sized SiC as compared with
281.2 MPa for pure copper. While, maximum hardness value
was determined as 87 HRB for 4 wt% nano SiC reinforced
nanocomposite as compared with 69 HRB for pure copper
sample. Wear resistance of the composite and nanocomposite
materials has been increased, and 4 wt% nano SiC reinforced
nanocomposite material displayed better wear resistance
among all samples. Optical microscopic images revealed bet-
ter grain refinement of composite/nanocomposite materials as
compared with pure copper sample. Scanning electron
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microscopic images confirmed uniform dispersion/
distribution of micro sized SiC/nano sized SiC in the copper
matrix.
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