Sanjay Kumar Thakur

Delphi Automotive Systems Singapore Pte Ltd.,

501 Ang Mo Kio Industrial Park 1,
Singapore 569621
e-mail: sanjay.kumar.thakur@delphi.com
K. Balasubramanian
Nonferrous Materials Technology Development
Centre,
Kanchanbagh, Hyderabad 500058,
India
e-mail: director@nftdc.res.in
Manoj Gupta
1
Department of Mechanical Engineering,
Faculty of Engineering,
National University of Singapore,
9 Engineering Drive 1,
Singapore 117576
e-mail: mpegm@nus.edu.sg
Microwave Synthesis and
Characterization of Magnesium
Based Composites Containing
Nanosized SiC and Hybrid SiC
+Al
2
O
3
Reinforcements
In the present study, monolithic magnesium, nanosized SiC reinforced magnesium and
nanosized hybrid SiC+Al
2
O
3
reinforced magnesium materials have been synthesized
by using powder metallurgy route involving microwave sintering followed by hot extru-
sion. The results show that the monolithic and the reinforced magnesium materials have
minimal porosity and the reinforced magnesium materials have fairly well distributed
nanosized SiC and SiC+Al
2
O
3
particles in the matrix. The thermo-mechanical property
measured in terms of coefcient of thermal expansion of the reinforced magnesium shows
dimensionally more stable magnesium as compared to monolithic magnesium. The hard-
ness 0.2% YS and UTS were found to improve signicantly after addition of nanosized
SiC and nanosized hybrid SiC+Al
2
O
3
particles to the magnesium, However, ductility
measured in terms of failure strain was found to be marginally reduced. Fractography
results showed the presence of brittle failure mode with cleavage steps on the fractured
surface of the magnesium matrix. DOI: 10.1115/1.2400279
Keywords: hybrid composites, nanocomposites, magnesium, mechanical properties, co-
efcient of thermal expansion
1 Introduction
Metal matrix composites MMCs consist of at least two phases
which can be totally different with respect to their physical prop-
erties. One phase is normally the metallic matrix and the second
phase is the reinforcement. The minimum requirement for the
combination of these phases in order to manufacture the MMCs is
the chemical afnity that leads to the formation of strong matrix
reinforcement interface. The loads and stresses are transferred
through the interface between the two phases. The interface plays
an important role for mechanical properties as well as for other
properties required for different applications 13.
Currently, light metal automotive applications are the focus of
interest due to the increasing cost of transportation. On one hand,
the necessity of reducing environmental pollution by lowering
fuel consumption and exhaust gases and on the other hand, pro-
tecting our natural resources has led to a renaissance in the use of
magnesium and its alloys in automotive industries 4. The pre-
requisites for establishing magnesium materials in automotive en-
gineering are low coefcient of thermal expansion CTE and bet-
ter mechanical properties. Newly developed magnesium alloys
serve these expectations partially. Moreover, magnesium alloy de-
velopment has reached its limit 5. Hence, magnesium matrix
composites are expected to have a big potential to substitute some
of the alloys, especially aluminum alloys, currently used in auto-
motive applications.
In the past, various types of reinforcements have been used in
the Mg matrix to produce composites having higher strength;
however, the ductility of the magnesium has been reported to be
adversely affected by the presence of ceramic reinforcements
2,6. It has been reported that the use of nanosized reinforce-
ments in the Mg matrix promises to affect the ductility favorably
as compared to those of micron sized reinforcements 7. There
have been reports on the use of nano-SiC 8,9 and nano-Al
2
O
3
10,11 reinforcements individually in the Mg matrix. However,
the nano-SiC and nano-Al
2
O
3
have not been used together as
hybrid reinforcement in the Mg matrix. Recently 5,1216, there
has been a renowned interest in using hybrid reinforcements in the
magnesium matrix to complement the properties of two or more
different reinforcements. The hybrid reinforcement, in general, is
a mixture of particles, whiskers, short bers, or combination of
these materials. By using hybrids, it is possible to have material
properties that could not have been obtained by using only one
type of reinforcement.
For producing MMCs, a number of processes have been intro-
duced that can broadly be categorized in two main processes, viz.,
powder metallurgy PM and ingot metallurgy IM techniques.
Ingot metallurgy is presently widely used for producing Mg
MMCs and is more relevant than the powder metallurgy route.
However, the advent of innovative, less expensive, cleaner, and
efcient processes, such as microwave synthesis 1719 of pow-
der compacts, has rejuvenated the interest in powder metallurgy
techniques once again to produce MgMMCs with improved
physical and mechanical properties as compared to those obtained
by using conventional heating. In conventional heating, the direc-
tion of heating is from outside to inside of the powder compact,
while for microwaves, the direction of heating is from inside to
outside of the powder compact. The former mode of heating re-
sults in poor microstructural characteristics of the core of the pow-
der compact while the latter results in poor microstructural char-
acteristics of the surface 20. To overcome the drawbacks of
these two ways of sintering, a combined action of microwaves and
microwave-coupled external heating source can be utilized to re-
1
Corresponding author.
Contributed by the Materials Division of ASME for publication in the JOURNAL OF
ENGINEERING MATERIALS AND TECHNOLOGY. Manuscript received January 24, 2006;
nal manuscript received June 17, 2006. Review conducted by Assimina Pelegri.
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alize rapid sintering from both inside and outside of the powder
compact 21,22. Moreover, SiC is a well known microwave sus-
ceptor material, hence incorporation of nano-SiC as a reinforcing
material may further assist in heating and sintering the powder
compacts of Mg and Al
2
O
3
. When microwaves are used to sinter
compacts, the time required to reach the sintering temperature and
the time of sintering are very small. Hence, the use of microwaves
provides less opportunity to form interfacial reaction products and
the grain growth to occur in the matrix. It is well known that
diffusion is a time and temperature dependent phenomenon.
Hence, by taking advantage of the fact that the microwave syn-
thesis of powder compacts can be realized in a shorter period of
time and at higher temperature 22, MMCs with superior proper-
ties can be produced. Moreover, microwave synthesized Mg com-
pacts having hybrid reinforcements, further promises to provide
superior properties as compared to conventionally singular rein-
forced Mg matrix composites.
There has been no report on using nanosized SiC and Al
2
O
3
together as a hybrid reinforcement in the Mg matrix to produce
composites by using two-directional microwave assisted synthesis
through the PM route. Hence, in the present study, an attempt has
been made to synthesize nanosized hybrid SiC and Al
2
O
3
rein-
forced Mg matrix composites by using a combination of the mi-
crowave assisted PM technique. To compare the properties of the
Mg/ SiC+Al
2
O
3
hybrid composites, monolithic Mg and
Mg/ SiC formulations were also prepared with the same process.
Further, the monolithic Mg, Mg/ SiC, and Mg/ SiC+Al
2
O
3
ma-
terials were hot extruded and characterized for physical, thermo-
mechanical, and mechanical properties to understand the viability
of the process and the materials considered under present investi-
gation. Particular emphasis was placed on investigating the sys-
tematic hybridization of nano-SiC particulates by using Al
2
O
3
particulates in nanolength scale.
2 Experimental Details
2.1 Materials. Magnesium powder used as matrix material in
the present investigation was procured from Merck, Germany and
was of 98.5% purity and in a size range of 60300 m. SiC and
Al
2
O
3
powder each with an average size of 50 nm, obtained from
Nanostructured & Amorphous Materials Inc. and Baikowski,
USA, respectively, were used as reinforcing materials.
2.2 Primary processing. The composite materials in the
present study were fabricated by using the powder metallurgy
technique. The raw materials were weighed and blended by using
RETSCH Planetary Ball Mill PM 400 at 200 rpm for 60 min. The
blended material was then compacted at a pressure of 50 tons to
form billets of 35 mm in diameter. The billets were then sintered
by using two-directional microwave assisted sintering. The com-
pacted billet was placed in a graphite crucible, surrounded by
silicon carbide powder and Fiberfrax insulation. The SiC powder
was used as susceptor material during microwave sintering as it
couples well with the microwave and absorbs microwave energy
readily and converts the microwave energy to heat. The crucible
containing the compacted billet was then placed in a Sharp micro-
wave oven for 27 min at 100% power for sintering. Microwaves
assisted the sintering from the insideoutside direction, while SiC
as the susceptor material assisted in sintering from the outside
inside direction as shown in Fig. 1.
2.3 Secondary Processing. To carry out the secondary pro-
cessing of as-sintered materials, the compacted billets were
soaked in a resistance furnace at a temperature of 400C for 1 h
followed by hot extrusion at 350C with an extrusion ratio of
25:1 producing rods of 7 mm in diameter. Extrusion was per-
formed by using a 150 ton hydraulic press with the help of col-
loidal graphite as lubricant. The extruded rods were subsequently
machined to different sizes for various characterization studies.
2.4 Physical Property Measurements. The density measure-
ments were performed on polished samples of magnesium and its
composites by using Archimedes principle 23. The porosity of
the samples was calculated by using the mass fraction of SiC and
Al
2
O
3
, and theoretical and experimental densities of the compos-
ite samples. The CTE of magnesium and its composite samples
were determined by using an automated Setaram 92-16/ 18
thermo-mechanical analyzer that used a spherical alumina probe
of 5 mm diameter. The test was conducted according to ASTM
E831-00 standard. The displacement of monolithic magnesium
and its composite samples was measured within a temperature
range of 50400C with a ramp rate of 5C/ min in an argon
atmosphere to determine the CTE of the samples. The Setaram
software was used to calculate the average CTE of the samples.
2.5 Microstructural Characterization. The microstructural
characterization of the extruded monolithic magnesium and its
composites were conducted in order to determine the size and
shape of grains, morphological characteristics of grains, and the
distribution of SiC and Al
2
O
3
particles in the magnesium matrix.
Microstructural characterization and the determination of distribu-
tion of the nanosized reinforcements in the magnesium matrix was
carried out by using an Hitachi S4100 eld emission scanning
electron microscope FESEM. The grain size and morphology of
the magnesium samples were determined by using an optical mi-
croscope Olympus BH2-UMA. The magnesium samples were
polished and etched by using acetic glycol 1.0 mL nitric acid,
19.0 mL distilled water, 20.0 mL acetic acid, and 60 mL ethylene
glycol to reveal the grain boundaries. The optical images ob-
tained were analyzed by using Scion Image Analyzer software.
X-ray diffraction studies were carried out on extruded samples of
pure magnesium and its composites by using an automated Shi-
madzu LAB-X XRD-7000 diffractometer with Cu K radiation by
using a scanning speed of 2 deg/ min.
2.6 Mechanical Characterization. The microhardness mea-
surements were carried out to investigate the inuence of the ad-
dition of nanosized SiC and Al
2
O
3
particles on the microhardness
of the magnesium matrix. The microhardness measurements were
performed by using Matsuzawa MXT50 automatic digital micro-
hardness tester attached with a Vickers indenter. The microhard-
ness test was performed according to ASTM E384-99 standard at
a test load of 25 gf for a dwell time of 15 s. The reinforcements of
50 nm in size were too small to perform an indentation test. Fur-
ther, the macrohardness of the samples was determined by using
Future-Tech FR-3 Rockwell type tester attached with Rockwell
15T supercial scale. The macrohardness tests were performed by
using a 1.588 mm ball indenter by applying a test load of 15 kgf
for 2 s according to ASTM E18-92 standard.
The tensile tests were conducted on round tensile specimens of
5 mm diameter and 25 mm gauge length of the extruded magne-
sium and its composites according to ASTM E8M-01 standard by
using MTS at an initial strain rate of 0.254 mm/ min. The frac-
tured samples obtained after tensile tests were used to carry out
Fig. 1 Schematic diagram showing the experimental setup
used in the present study
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fractography study of monolithic magnesium and its composites
to provide an insight into the fracture mechanism which were
operative during tensile loading. The fractography studies were
carried out by using a JEOL JSM-5600LV SEM.
3 Results and Discussion
3.1 Processing and Macrostructure. The powder metallurgy
technique was successfully employed for the fabrication of mono-
lithic magnesium and its hybrid nanocomposites. One of the fac-
tors that determines the properties of the composites prepared
through the PM technique is the clustering of the blended pow-
ders. It was observed that after blending, there were no visible
clusters, hence showing the effective blending during processing
that provided even distribution of the powders. Minimal surface
damage was observed on the extruded rods because of the suitable
parameters chosen for extrusion of the monolithic Mg and hybrid
Mg nanocomposites. The results of the density and the porosity
measurements are summarized in Table 1. The percentage of po-
rosity was calculated from the experimental and theoretical den-
sity values. The experimental densities determined by
Archimedes principle were closer to the theoretically calculated
values based on rule of mixture indicating low porosity levels see
Table 1. The results show that the density of the Mg increased
marginally after addition of nanosized reinforcements of 1% SiC.
However, when Mg/ SiC formulation was hybridized by an in-
creasing presence of nanosized Al
2
O
3
reinforcement, the effect
was to decrease marginally the density of Mg/ SiC accompanied
by a marginal increase in porosity of the samples. It is clear from
the ndings that the increase in porosity is more sensitive to the
addition of Al
2
O
3
nanoparticles as compared to that of nano-SiC.
The presence of the minimal porosity can be attributed to the
appropriate selection of compaction, sintering, and extrusion pa-
rameters and also to good compatibility between the magnesium
matrix and the reinforcements.
3.2 Microstructural Characterization. The results of the
grain morphology determination are summarized in Table 2. The
analysis of extruded specimens by using optical microscope re-
vealed predominantly equiaxed grain structure indicating that the
extrusion temperature chosen was sufcient to allow the recrys-
tallization of strain-free grains upon extrusion. As compared to the
monolithic magnesium, the composites showed a general reduc-
tion in grain size. The effect of addition of Al
2
O
3
seems to be
more predominant than that of SiC on the grain size reduction of
the magnesium matrix. The grain renement effect can be attrib-
uted to: a the increase in the constraint to grain growth because
of the presence of nanosized reinforcements 24; b the capabil-
ity of nano sized SiC and Al
2
O
3
particles to nucleate magnesium
grains during recrystallization 25; c use of microwave sintering
that may assist in preventing grain growth due to less time avail-
able at sintering temperature; and d suitable hot extrusion
parameters.
The FESEM was utilized to assess the overall distribution of
nanosized reinforcements in the matrix. FESEM micrographs re-
vealed that the distribution of SiC particles in the Mg/ 1%SiC
composite is relatively uniform. Similarly, the distribution of re-
inforcements in the hybrid SiC+Al
2
O
3
reinforced Mg compos-
ites also appeared to be uniform see Figs. 2a2c. This im-
plies that the combination of blending and extrusion parameters
chosen were suitable for fabrication of the nanocomposites of Mg.
However, as the FESEM was not equipped with an energy disper-
sive X-ray EDX facility, it was not possible to differentiate be-
tween SiC and Al
2
O
3
nanoparticles. In addition, it was difcult to
assess the interfacial integrity between the reinforcements and the
matrix due to the small size of the reinforcement particles. To
conrm the various phases in the composite materials, x-ray dif-
fraction XRD studies were conducted. The XRD results con-
rmed the presence of Mg phase in pure Mg and its composites.
However, the presence of reinforcements could not be detected
due to the limitation of the XRD to detect phases less than
2 vol % 26. The possible interfacial reactions that may occur at
the interface between the matrix and the reinforcements used in
the present investigation are described by Eqs. 15 4,27,28
2Mg + O
2
= 2MgO G = 569 kJ/mol 1
3Mg + 4Al
2
O
3
= 3MgAl
2
O
4
+ 2Al G = 231 kJ/mol 2
2Mg + SiC = Mg
2
Si + C G = 145 kJ/mol 3
3Mg + Al
2
O
3
= 3MgO + 2Al G = 126 kJ/mol 4
MgO + Al
2
O
3
= MgAl
2
O
4
G = 33 kJ/mol 5
However, during XRD studies, no peaks were detected for any of
the above-mentioned phases, probably because of the small
amount of reinforcements. There may be a very small amount of
interfacial products, especially MgO, MgAl
2
O
4
, and Mg
2
Si ac-
cording to Eqs. 13, respectively. It may be noted that the free
energy of reaction, G, is the lowest for Eq. 1 followed by Eqs.
2 and 3 that favors the aforementioned reactions to occur at the
interface between the reinforcements and the magnesium matrix.
3.3 Coefcient of Thermal Expansion. To understand the
thermo-mechanical behavior of the monolithic Mg and its com-
posites, dilatometric tests were carried out in the temperature
range of 50400C and CTE values were measured for each
sample. For comparison purposes, theoretical CTE values of Mg
composites were computed by using the rule-of-mixture ROM
model 29 as expressed by Eq. 6
=
m
V
m
+
r
V
r
6
where and V represent CTE and volume fraction of the phase,
respectively, while the subscripts m and r refer to the matrix and
the reinforcement, respectively. By using the values of
Mg
=29.3310
6
/ C,
SiC
=4.310
6
/ C 30, and
Al
2
O
3
=7.4
10
6
/ C 31, the theoretical CTEs of the MMCs were com-
puted and summarized in Table 3.
The experimental results of CTE measurements revealed that
the presence of SiC and Al
2
O
3
reinforcements reduced the aver-
age CTE value of the magnesium matrix and caused a noticeable
increase in dimensional stability of the Mg matrix see Table 3.
The average CTE value was found to be lowest for Mg composite
Table 1 Results of density and porosity measurements
Materials
Theoretical
density
g/ cm
3

Experimental
density
g/ cm
3

Porosity
%
Pure Mg 1.740
1.73450.0017 0.3170.097
Mg+1% SiC 50 nm
1.748
1.74140.0007 0.3790.038
Mg+0.5% SiC 50 nm
+0.5% Al
2
O
3
50 nm
1.749
1.74100.0006 0.4360.034
Mg+0.3% SiC 50 nm
+0.7% Al
2
O
3
50 nm
1.749
1.74070.0009 0.4660.052
Table 2 Results of grain size and morphology
Materials Grain size Aspect ratio Roundness
Pure Mg
29.921.91 1.140.32 1.550.43
Mg+1% SiC 50 nm 28.711.52 1.560.61 1.690.87
Mg+0.5% SiC 50 nm
+0.5% Al
2
O
3
50 nm
26.271.56 1.790.57 1.440.32
Mg+0.3% SiC 50 nm
+0.7% Al
2
O
3
50 nm
25.791.87 1.850.53 1.630.38
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containing 0.3%SiC+0.7%Al
2
O
3
. The highest CTE value was
for pure Mg followed by Mg/ 1%SiC composite and
Mg/ 0.5%SiC+0.5%Al
2
O
3
composites. Again, it is clear that the
presence of nanosized Al
2
O
3
is more effective in reducing the
CTE value of Mg as compared to nanosized SiC particles. The
lowering of the CTE value of the Mg in the presence of SiC and
Al
2
O
3
particles can be attributed to: a the lower CTE values of
SiC 4.310
6
/ C and Al
2
O
3
7.410
6
/ C reinforcements
as compared to that of the Mg 29.3310
6
/ C matrix; b uni-
form distribution of the reinforcements in the matrix; and c the
fact that the presence of ceramic reinforcements with good inter-
facial integrity impedes the matrix from expanding during thermal
ramping 32. From Table 3, it is clear that the experimental val-
ues of CTE were lower than the theoretical values. This can be
due to the coupled effect of: a the uniform distribution of nano-
SiC and nano-Al
2
O
3
particles and b good interfacial integrity
between the reinforcements and the Mg matrix. It is believed that
the contribution of nanoreinforcement particles may be subverted
by the presence of porosity in the matrix 11.
3.4 Mechanical Characterization. The mechanical behavior
of the extruded samples of monolithic magnesium and its com-
posites was assessed in terms of their microhardness, macrohard-
ness, and tensile properties. The results of the macrohardness
measurements see Table 4 revealed that there was an increasing
trend in the macrohardness values measured on the magnesium
matrix as the reinforcements were added. From Table 4, it is clear
that the matrix macrohardness was highest for Mg+0.3%SiC
+0.7%Al
2
O
3
10.45% increase as compared to pure Mg compos-
ite followed by Mg+0.5%SiC+0.5%Al
2
O
3
8.54% increase as
compared to pure Mg, Mg+1% SiC 5.7% increase as compared
to pure Mg, and pure Mg. The increase in macrohardness of the
matrix with the addition of the reinforcements can be due to: a
the presence of harder SiC and Al
2
O
3
particles as reinforcements
and b reduced grain size of the matrix.
A similar trend in increase in microhardness of the matrix was
observed when 1%SiC, 0.5%SiC+0.5%Al
2
O
3
, and 0.3%SiC
+0.7%Al
2
O
3
were added to the Mg matrix in the order mentioned
above. The higher microhardness for composites as compared to
monolithic magnesium may be attributed to: a the presence of
relatively harder ceramic particles in the matrix; b constraints on
localized matrix deformation during indentation due to the pres-
ence of reinforcements; and c the presence of reduced grain size
33. The hardness results obtained in the present study are similar
to the ndings reported for nanosized ceramic reinforced magne-
sium matrix 11. It may be noted that the microhardness measure-
ments provide a better indication of the effects of the reinforce-
ments on the matrix as the measurements are taken at specic
Fig. 2 Representative FESEM micrographs showing the distri-
bution of: a SiC in Mg/ 1%SiC; b SiC and Al
2
O
3
in
Mg/ 0.5%SiC+0.5%Al
2
O
3
; and c SiC and Al
2
O
3
in
Mg/ 0.3%SiC+0.7%Al
2
O
3
composites
Table 3 Results of CTE measurements
Materials
Average CTE
10
6
/ C
Theoretical CTE, ROM model
10
6
/ / C
Pure Mg
29.330.72

Mg+1% SiC 50 nm 27.990.69
29.20
Mg+0.5% SiC 50 nm
+0.5% Al
2
O
3
50 nm
27.560.71
29.22
Mg+0.3% SiC 50 nm
+0.7% Al
2
O
3
50 nm
26.730.45
29.21
Table 4 Results of hardness measurements
Materials
Matrix Microhardness
HV
Matrix Macrohardness
HR15 T
Pure Mg
39.080.82 43.321.68
Mg+1% SiC 50 nm 43.080.71 45.821.22
Mg+0.5% SiC 50 nm
+0.5% Al
2
O
3
50 nm
46.120.94 47.020.96
Mg+0.3% SiC 50 nm
+0.7% Al
2
O
3
50 nm
47.960.51 47.850.59
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points free of defects, which may affect the results.
In order to understand the mechanical behavior of the Mg com-
posites, tensile tests were conducted and 0.2% YS and UTS of the
composite materials were determined and tabulated in Table 5.
From the results in Table 5, it is clear that the addition of nano-
sized ceramic reinforcements to the Mg matrix signicantly im-
proved the 0.2% YS and UTS values; however, the ductility mea-
sured in terms of failure strain was marginally affected. The
addition of 1%SiC to Mg increased its 0.2% YS by about 10%,
whereas, hybridization of the Mg matrix by adding 0.5%SiC
+0.5%Al
2
O
3
increased the 0.2% YS of Mg by 30.37%. Similarly,
by increasing the amount of Al
2
O
3
to 0.7% and decreasing the
amount of SiC to 0.3% keeping the total weight percent of rein-
forcement at a constant level of 1% increased the 0.2% YS of Mg
by 38.12%, an increase in 0.2% YS by 5.94% as compared to Mg
containing 0.5%SiC+0.5%Al
2
O
3
. However, the 0.2% YS of Mg
containing 0.5%SiC+0.5%Al
2
O
3
increased by 18.69% as com-
pared to Mg containing 1% SiC. Hence, it can be said that hybrid-
ization of Mg/ 1%SiC composite by adding Al
2
O
3
further in-
creased the 0.2% YS of Mg; however, further increase in the
amount of Al
2
O
3
did not increase the 0.2% YS of Mg signi-
cantly. A similar trend in increase in UTS of Mg was found when
SiC and Al
2
O
3
were added to it as shown in Table 5. The highest
UTS was recorded for Mg/ 0.3%SiC+0.7%Al
2
O
3
composite fol-
lowed by Mg/ 0.5%SiC+0.5%Al
2
O
3
and Mg/ 1%SiC compos-
ites with an increase in UTS by 21.8%, 16.64%, and 7.78%, re-
spectively, as compared to the monolithic Mg. The increase in
strength of the Mg matrix after addition of reinforcing particles
can be due to: a the increase in grain boundary area due to grain
renement 24,34; b the strong multidirectional thermal stress
at the reinforcement-matrix interface with grain boundaries in-
duced by the large difference between the CTE values of the ma-
trix and the reinforcements 35,36; and c the effective transfer
of applied tensile load to the uniformly distributed and well
bonded reinforcements.
The results of the tensile test revealed that the failure strain
marginally decreased with the addition of reinforcements. This is
in agreement with the results reported elsewhere 2, when it was
found that the addition of reinforcing particles caused a reduction
in the tensile elongation. The addition of Al
2
O
3
caused a greater
decrease in failure strain as compared to SiC. Hence, it can be said
that to obtain an optimum advantage of nanosized particles of SiC
and Al
2
O
3
hybridization in the Mg matrix, 0.5% SiC combined
with 0.5% Al
2
O
3
provides the best combination of strength and
ductility.
The results of fracture analysis revealed typical brittle fracture
Fig. 3 Representative SEM micrographs showing the fractured surface of: a pure Mg; b Mg/ 1%SiC composite; c
Mg/ 0.5%SiC+0.5%Al
2
O
3
composite; and d Mg/ 0.3%SiC+0.7%Al
2
O
3
composites
Table 5 Results of tensile testing
Materials
0.2% YS
MPa
UTS
MPa
Failure strain
%
Pure Mg
119.397.63 169.224.40 5.471.57
Mg+1% SiC 50 nm 131.1412.33 182.409.43 5.010.46
Mg+0.5% SiC 50 nm
+0.5% Al
2
O
3
50 nm
155.666.99 197.381.83 4.582.08
Mg+0.3% SiC 50 nm
+0.7% Al
2
O
3
50 nm
164.911.43 206.105.28 4.171.78
198 / Vol. 129, APRIL 2007 Transactions of the ASME
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in the magnesium matrix see Fig. 3a with the presence of
cleavage step. This can be attributed to the hexagonal closed
packed crystal structure of the magnesium, which restricts the slip
to occur only at the basal plane 24. The presence of small steps
and microscopically rough structure indicates the inability of mag-
nesium to cleave on any single plane. Due to the limitations of the
SEM, it was not possible to obtain the microstructure of the SiC
and Al
2
O
3
particles after fracture. The composites showed a mi-
croscopically rough surface see Figs. 3a3d with the pres-
ence of relatively smaller cleavage steps. The presence of a rela-
tively smaller step can be attributed to the presence of SiC or
SiC+Al
2
O
3
particles. Further work is continuing in this area.
4 Conclusions
1. It is possible to synthesize magnesium based composites
containing nanosized SiC and Al
2
O
3
hybrid reinforcements
by the microwave assisted powder metallurgy route coupled
with hot extrusion.
2. The primary and secondary processing parameters used in
the present investigation are suitable to produce monolithic
Mg, Mg/nano-SiC, and nanosized hybrid reinforced SiC
+Al
2
O
3
Mg composites with ne and equiaxed grains, rea-
sonably uniform distribution of reinforcements, and minimal
porosity.
3. The nano-SiC reinforced and nanohybrid SiC+Al
2
O
3
re-
inforced magnesium were dimensionally more stable than
monolithic magnesium according to the results of the CTE
measurements.
4. The addition of nano-SiC and nano-SiC+Al
2
O
3
hybrid re-
inforcements to the Mg matrix led to signicant increase in
hardness, 0.2% YS, and UTS, whereas ductility measured in
terms of failure strain was marginally reduced.
5. The brittle mode of failure was observed on the fractured
Mg matrix surface with the presence of cleavage steps.
Acknowledgment
The authors thank Ajitha Ram for her assistance during the
course of the present investigation. The authors also thank Na-
tional University of Singapore Grant No. R-265-000-169-112
and Delphi Automotive Systems Singapore Pte Ltd for providing
assistance during preparation of the manuscript.
References
1 Rohatgi, P. K., Asthana, R., and Das, S., 1986, Solidication, Structures, and
Properties of Cast Metal-Ceramic Particle Composities, Int. Met. Rev., 31,
pp. 115139.
2 Lloyd, D. J., 1994, Particle Reinforced Aluminum and Magnesium Matrix
Composites, Int. Mater. Rev., 39, pp. 123.
3 Luo, A., 1995, Processing, Microstructure and Mechanical Behaviour of Cast
Magnesium Metal Matrix Composites, Metall. Trans. A, 26A, pp. 2445
2455.
4 Hort, N., Dieringa, H., Thakur, S. K., and Kainer, K. U., 2006, Magnesium
Matrix Composites, Magnesium Technology: Metallurgy, Design Data, Appli-
cations, H. E. Friedrich and B. L. Mordike, eds., Springer-Verlag, Berlin, pp.
315334.
5 Schroder, J., and Kainer, K. U., 1991, Magnesium-Base Hybrid Composites
Prepared by Liquid Inltration, Mater. Sci. Eng., A, 135, pp. 3336.
6 Everette, R. K., and Arsenault, R. J., eds., 1991, Metal Matrix Composites:
Processing and Interfaces, Academic, New York, p. 228.
7 Goh, C. S., Wei, J., Lee, L. C., and Gupta, M., 2006, Development of Novel
Carbon Nanotube Reinforced Magnesium Nanocomposites Using the Powder
Metallurgy Technique, Nanotechnology, 17, pp. 712.
8 Lan, J., Yang, Y., and Li, X., 2004, Microstructure and Microhardness of SiC
Nanoparticles Reinforced Magnesium Composites Fabricated by Ultrasonic
Method, Mater. Sci. Eng., A, 386, pp. 284290.
9 Ferkel, H., and Mordike, B. L., 2001, Magnesium Strengthened by SiC Nano-
particles, Mater. Sci. Eng., A, 298, pp. 193199.
10 Trojanova, Z., Lukac, P., Ferkel, H., Mordike, B. L., and Riehemann, W.,
1997, Stability of Microstructure in Magnesium Reinforced by Nanoscaled
Alumina Particles, Mater. Sci. Eng., A, 234236, pp. 798801.
11 Hassan, S. F., and Gupta, M., 2004, Development of High Performance Mag-
nesium Nanocomposites Using Solidication Processing Route, Mater. Sci.
Technol., 20, pp. 13831388.
12 Thakur, S. K., Dhindaw, B. K., Hort, N., and Kainer, K. U., 2004, Some
Studies on Thermal Expansion Behavior of C-Fiber, SiCp and Mg
2
Si In-Situ
Reinforced AZ31 Mg-Alloy Based Hybrid Composites, Metall. Mater. Trans.
A, 35A, pp. 11671176.
13 Kumar, S. R., Panigrahi, M. K., Thakur, S. K., Kainer, K. U., Chakraborty, M.,
and Dhindaw, B. K., 2006, Characterization of Stress in Reinforcements in
Magnesium Based Squeeze Inltrated Cast Hybrid Composites, Mater. Sci.
Eng., A, 415, pp. 207212.
14 Gu, J., Zhang, X., and Gu, M., 2004, Mechanical Properties and Damping
Capacity of SiCp+Al
2
O
3
SiO
2
f / Mg Hybrid Metal Matrix Composite, J.
Alloys Compd., 385, pp. 104108.
15 Gu, M., Wu, Z., Jin, Y., and Kocak, M., 1999, Effects of Reinforcements on
the Aging Response of a ZK60-based Hybrid Composite, Mater. Sci. Eng., A,
272, pp. 257263.
16 Thakur, S. K., Dieringa, H., Dhindaw, B. K., Hort, N., and Kainer, K. U.,
2005, Thermal Cycling and Creep Studies of AM50+Nd Magnesium Alloy
Based Carbon Fiber, SiC particulate and In-Situ Mg
2
Si Reinforced Hybrid
Composites, Transactions of the Indian Institute of Metals, 58, pp. 653659.
17 IFAM Dresden Invests in Microwave Sintering for Metals, 2003, Powder
Metall., 46, pp. 191191.
18 Anklekar, R. M., Bauer, K., Agrawal, D. K., and Roy, R., 2005, Improved
Mechanical Properties and Microstructural Development of Microwave Sin-
tered Copper and Nickel Steel PM Parts, Powder Metall., 48, pp. 3946.
19 Breval, E., Cheng, J. P., Agrawal, D. K., Gigl, P., Dennis, A., Roy, R., and
Papworth, A. J., 2005, Comparison Between Microwave and Conventional
Sintering of WC/ Co Composites, Mater. Sci. Eng., A, 391, pp. 285295.
20 Roy, R., Cheng, J., and Agrawal, D., 2002, US Patent No. 6,365,885 B1.
21 Wong, W. L. E., Karthik, S., and Gupta, M., 2005, Development of High
Performance MgAl
2
O
3
Composites Containing Al
2
O
3
in Submicron Length
Scale using Microwave Assisted Rapid Sintering, Mater. Sci. Technol., 21,
pp. 10631070.
22 Gupta, M., and Wong, W. L. E., 2005, Enhancing Overall Mechanical Per-
formance of Metallic Materials using Two-directional Microwave Assisted
Rapid Sintering, Scr. Mater., 52, pp. 479483.
23 Gupta, M., Srivatsan, T. S., Mohamed, F. A., and Lavernia, E. J., 1993, Mi-
crostructural Evolution and Mechanical Properties of SiC/ Al2O
3
Particulate
Reinforced Spray Deposited Metal Matrix Composites, J. Mater. Sci., 28, pp.
22452259.
24 Reed-Hill, R. E., 1964, Physical Metallurgy Principles, D. Van Nostrand Com-
pany, New York, pp. 192194, 267, 753.
25 Shewmon, P. G., 1969, Transformation in Metals, McGraw-Hill, New York,
pp. 69.
26 Cullity, B. D., 1978, Elements of X-Ray Diffraction, Addison-Wesley, Reading,
Massachusetts, pp. 414.
27 Kubaschewski, O., and Alcock, C. B., 1979, Metallurgucal Thermichemistry,
Pergamon, Oxford, UK.
28 Barin, I., 1989, Thermochemical Data of Pure Substances, VCH-
Verlagsgesellschaft, Weinheim, Germany.
29 Vaidya, R. U., and Chawla, K. K., 1994, Thermal Expansion of Metal-Matrix
Composites, Compos. Sci. Technol., 50, pp. 1322.
30 ASM Handbook, Engineering Materials, 6th ed., Budinski, Specication sheet,
ASM, Metals Park, Ohio.
31 Brandes, E. A., and Brook, G. B., eds., 1998, Smithells Metals Reference Book,
Butterworth-Heinemann, London, pp. 512.
32 Wai, L. K., 2003, Development of new aluminum based hybrid composites,
B. Eng. thesis, National University of Singapore, Singapore, 2003, pp. 152.
33 Arsenault, R. J., and Shi, N., 1986, Dislocation Generation Due to Differ-
ences Between the Coefcients of Thermal Expansion, Mater. Sci. Eng., 81,
pp. 175187.
34 Murr, L. E., 1975, Interfacial Phenomena in Metals and Alloys, Addison-
Wesley, Reading, Massachusetts, pp. 202208, 340344.
35 Geiger, A. L., and Walker, J. A., 1991, The Processing and Properties of
Discontinuously Reinforced Aluminum Composites, JOM, August, pp. 815.
36 Ibrahim, I. A., Mohamed, F. A., and Lavernia, E. J., 1991, Particulate Rein-
forced Metal Matrix Composites: A Review, J. Mater. Sci., 26, pp. 1137
1156.
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