Original article

Proc IMechE Part L:

J Materials: Design and Applications
Phase, microstructure, and wear behavior 0(0) 1–14
! IMechE 2019
of Al2O3-reinforced Fe–Si alloy-based Article reuse guidelines:
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metal matrix nanocomposites DOI: 10.1177/1464420719893387

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Akash Saxena1, Neera Singh2, Bhupendra Singh3,

Devendra Kumar1, Kishor Kumar Sadasivuni4 and
Pallav Gupta5

Abstract
In the present work, phase, microstructure, and wear properties of Al2O3-reinforced Fe–Si alloy-based metal
matrix nanocomposites have been studied. Composites using 2 wt.% and 5 wt.% of Si and rest Fe powder mix were
synthesized via powder metallurgy and sintered at different temperature schedules. Iron–silicon alloy specimens were
found to have high hardness and high wear resistance in comparison to pure iron specimens. Addition of 5 wt.% and
10 wt.% alumina reinforcement in Fe–Si alloy composition helped in developing iron aluminate (FeAl2O4) phase in
composites which further improved the mechanical properties i.e. high hardness and wear resistance. Formation of
iron aluminate phase occurs due to reactive sintering between Fe and Al2O3 particles. It is expected that the improved
behavior of prepared nanocomposites as compared to conventional metals will be helpful in finding their use for wide
industrial applications.

Keywords
Metal matrix nanocomposites, alloys, powder metallurgy, X-ray diffraction, scanning electron microscopy, wear

Date received: 2 July 2019; accepted: 18 November 2019

deposition (CVD).5–7 Incorporation of fine ceramic

Introduction
New developments in metal matrix nanocomposites
(MMNCs) have been done for several years to fulfill
the current demand in technology of advanced struc-
tural applications. MMNCs are the candidates,
known for their high mechanical strength and good
corrosion resistance.1,2 These are made by the add-
ition of two or more physically distinct constituents
having different properties, but their combination
shows improved mechanical and electrochemical
properties as compared to the starting materials.3
Better MMNCs can only be manufactured by
choosing the optimum parameters such as compos-
ition, microstructure, degree of crystallinity, phase
distribution, crystallographic texture etc.4 Synthesis
process of a composite plays an important role to
alter the above parameters. Optimized synthesis
route increases the overall cost of a composite due
to increased complexity. Different manufacturing
methods commonly used for fabricating MMNC
are powder metallurgy (P/M), physical vapor depos-
ition (PVD), stir casting, and chemical vapor
particles in ductile metal or alloy matrix using
powder metallurgy (P/M) is a simple process which
helps in achieving the desired mechanical properties.
It also helps in increasing the resistance against envir-
onmental attack by improving corrosion resistance. P/
M is widely used as it makes use of less heat consump-
tion and helps in developing a homogenous product
with better physical, mechanical, and electrochemical
1
Department of Ceramic Engineering, Indian Institute of Technology
(Banaras Hindu University), Varanasi, India
2
Department of Mechanical and Industrial Engineering, Tallinn
University of Technology, Tallinn, Estonia
3
Light Weight Metallic Materials Division, CSIR–Advanced Materials
and Processes Research Institute, Bhopal, India
4
Center for Advanced Materials, Qatar University, Doha, Qatar
5
Department of Mechanical Engineering, Amity School of Engineering
and Technology, Amity University Uttar Pradesh, Noida, India
Corresponding author:
Pallav Gupta, Department of Mechanical Engineering, Amity School of
Engineering and Technology, Amity University Uttar Pradesh, Noida,
Uttar Pradesh 201313, India.
Email: pgupta7@amity.edu
2 Proc IMechE Part L: J Materials: Design and Applications 0(0)
properties.8,9 Various factors such as reinforcement
distribution, nature of reinforcement, its volume frac-
tion, and the interfacial reaction between matrix and
reinforcement are the important parameters which
should also be considered during synthesis.
Gupta et al. investigated the structural and mech-
anical behavior of Fe–Al2O3 MMNCs. Prepared com-
posites were reported to have homogenous property
distribution with less processing temperature utiliza-
tion. Initial powders were ball milled and then com-
pacted in cylindrical shapes which were then followed
by sintering in the range of 900–1100  C for 1–3 h in
an inert environment. Formation of iron aluminate
(FeAl2O4) was found to be responsible in the enhance-
ment of density, hardness, wear resistance and corro-
sion resistance.10,11
Jha et al. synthesized Fe–ZrO2 MMCs by P/M and
studied their structural and mechanical behavior. Five
to thirty weight percentage of zirconium dioxide was
added in the iron matrix, which was mixed using ball
mill and then compacted in cylindrical shaped die.
Sintering was done in an inert atmosphere at a tem-
perature range 900–1100  C for 1–3 h. Formation of
iron zirconium oxide (Zr6Fe3O) resulted as a result of
the reactive sintering between Fe and ZrO2 particles,
which was found to help in improving densification,
hardness, and wear resistance of the composite.12
Several studies have been reported based on the
synthesis and characterization of iron-based MMNC
using alumina (Al2O3), zirconium dioxide (ZrO2), and
silicon carbide (SiC) as reinforcement.13,14 A few more
studies have also been performed using dopants to
improve the mechanical and electrochemical charac-
teristics.15 However, there were no significant studies
found on iron–silicon alloy matrix and also when the
matrix is reinforced with alumina. Therefore, the pre-
sent paper is focused on the iron–silicon alloy-based
nanocomposites using alumina as reinforcement.
Experimental
Electrolytic Fe (99.5% pure, average size 49–58 mm),
Si (99% pure, 74 mm), and Al2O3 (63–210 mm) pow-
ders were used as initial powders. All the powders
were weighed using an electronic weighing balance
of accuracy 0.0001 g and ball milled using ZrO2
balls as grinding media. Powder to ball ratio of 1:2
Table 1. Different Fe–Si specimens and their processing conditions.
Composition (wt.%)
Sintering
Sample No. Iron (%) Silicon (%) temperature ( C)
1 95 5 1000
2 98 2 1100
3 98 2 1200
4 98 2 1200
was maintained during ball milling. Compaction of
mixed powders was done using a hydraulic press,
under uniaxial load of 9 tons. Green compacts were
sintered in a temperature range of 1000–1200  C
for different time intervals in argon atmosphere-con-
trolled furnace. A nomenclature, for example,
2SF1100(3) is given to prepared specimens where 2S
represents the amount (in wt.%) of Si, F represents
the amount of Fe, 1100 represents the temperature of
sintering, and (3) represents the sintering time in hours.
Similarly, another nomenclature 10A2SF1200(3) is
given for specimens where A, Si, and Fe are the
amount (in wt.%) of Al2O3, Si, and Fe, respectively,
whereas 1200 is temperature of sintering and 3
denotes sintering time in hours. Tables 1 and 5
illustrate the nomenclatures of each synthesized
specimen in detail.
Phase analysis of the sintered specimens was done
with the help of Rigaku Desktop Miniflex II X-Ray
diffractometer employing Cu–Ka radiation and Ni
filter. Acceleration voltage was 30 kV, acceleration
current as 15 mA, and step size of 0.02 was used in
the present research work. Grinding of the specimen
surfaces is done using different grades of emery papers
(320 mm; 600 mm; 1000 mm; 1200 mm; 1500 mm) and
finally polished using a diamond paste of size 1 mm.
Microstructure study was conducted with the help
of Evo 18 Zeiss scanning electron microscope
(SEM), equipped with energy-dispersive spectroscopy
(EDX). Hardness test was done using Rockwell hard-
ness tester with the help of 1/800 H scale steel ball
indenter at 60 kgf load. Wear test was performed
using a pin on disc (POD) wear testing machine at
three different loads. Fixed sliding distance (14.4 km)
and speed (4 km/h) were taken during the test.15
Weight loss after wear test was recorded for calculat-
ing the wear rate values. Total weight loss (g)
during this process was measured, by dividing to the
density and total distance covered by the sample.
Wear loss by the sample per km is given by the equa-
tion below.
Mass loss ðgÞ
Wear rate ¼ 8   9
< Sample density g =
cc
: Total distance travelled ðkmÞ ;
Sintering time Nomenclature
3 hours 5SF1000(3)
3 hours 2SF1100(3)
1 hours 2SF1200(1)
3 hours 2SF1200(3)
Saxena et al. 3

Fe–Si MMNC X-ray diffraction

Four different compositions of Fe–Si have been
prepared as listed in Table 1. A correlative study
between phase, microstructure, and mechanical
behavior of specimens is investigated with varying sin-
tering schedule and silicon content. Table 1 shows
different Fe–Si specimens and their processing
conditions.
X-ray diffraction (XRD) pattern of 5SF1000(3),
2SF1100(3), 2SF1200(1), and 2SF1200(3) specimens
is shown in Figure 1(a) to (d). Present phases, their
(h k l) values, and related JCPDS files are given in
Table 2. Presence of Fe and Si is observed in all the
patterns. In case of metals, diffusion between present
elements occurs as a result of solid-state diffusion.

Figure 1. XRD of (a) 5SF1000(3), (b) 2SF1100(3), (c) 2SF1200(1), and (d) 2SF1200(3).

Table 2. X-ray diffraction analysis.

S. No. Compound name Empirical formula (h k l) d-spacing (Å) XRD-JCPDS files

1 Iron Fe (1 1 0) 2.0300 01-1262

2 Fe (2 0 0) 1.4400
3 Iron aluminium oxide FeAl2O4 (3 1 1) 2.4597 34-0192
4 (2 2 0) 2.8830
5 (5 1 1) 1.5691
6 Iron silicon Fe–Si (2 2 2) 1.2891 76-1748
7 Silicon Si (1 1 1) 3.11307 80-0018
8 (2 2 0) 1.9063
9 (3 3 1) 1.2400 03-0534
10 Iron oxide Fe2O3 (1 0 4) 2.6814 84-0309
11 (1 1 0) 2.5190 73-0603
12 Iron–silicon oxide FeSiO3 (0 2 1) 3.3500 17-0548
13 Silicon oxide SiO2 (1 3 2) 1.7953 82-1561
14 (1 0 1) 4.0388 77-1316
15 (1 0 1) 3.1274 79-1915
16 Aluminium oxide Al2O3 (2 0 13) 1.4200 02-0921
4 Proc IMechE Part L: J Materials: Design and Applications 0(0)
Since the addition of Si is small, therefore, major
peaks of Fe are observed in all the patterns and
only a few minor peaks of Si can be seen.
Formation of a new phase Fe–Si is also evident as a
result of diffusion between Fe and Si metals in all the
specimens. Figure 1(a) shows the XRD pattern of
5SF1000(3). Presence of Fe, Si, and intermetallic com-
pound Fe–Si is observed in the pattern. Along with
these, a few minor peaks of Fe2O3 and SiO2 are also
observed which may be due to trap of oxygen during
sintering. From Figure 1(b), it is observed that the
intensity of Si and Fe–Si is reduced due to the less
concentration of Si i.e. 2% in specimen 2SF1100(3).
In Figure 1(c), the intensity of Fe–Si is slightly
increased due to the increased diffusion between Fe
and Si metals as a result of increased sintering tem-
perature for specimen 2SF1200(1). When the sintering
duration is increased upto 3 h for specimen
2SF1200(1), again an increase in the Fe–Si intensities
is observed which can be observed in Figure 1(d).
Therefore, it is concluded that content of Si, sintering
temperature, and sintering duration have increased
the formation of Fe–Si intermetallic compound due
to increased diffusion of elements.
Scanning electron microscopy
SEM images of well-polished specimen surfaces
of 5SF1000(3), 2SF1100(3), 2SF1200(1), and
2SF1200(3) at 500 magnification are shown in
Figure 2(a) to (d). Obtained micrographs show the
grain size, their distribution, and densification behav-
ior in the specimens. Confirmation of present elements
is evident from the EDX analysis (Figures 3–6).
Uniform distribution of phases in the 5SF1000(3)
specimen can be observed in the micrograph 2(a) with
nanosize grains starting from 260 nm onwards. Along
with this, the presence of pores can also be observed.
These pores may be generated due to the improper
bonding between Fe and Si.16 During sintering for
specimen having high Si content, it has resulted in
the brittle behavior of Fe–Si specimens. From
Figure 2(b), micrographs show that complete densifi-
cation has not occurred in 2SF1100(3) at 1100  C tem-
perature. Therefore, the presence of defects can be
Figure 2. SEM of (a) 5SF1000(3), (b) 2SF1100(3), (c) 2SF1200(1), and (d) 2SF1200(3) at 500 magnification.
observed in the microstructure. SEM micrograph of
2SF1200(1) in Figure 2(c) shows a well dense micro-
structure resulting from complete diffusion of Fe and
Si. The presence of a very less amount of pore volume
as compared to specimen 5SF1000(3) and 2SF1100(3)
is evident in Figure 2(c). With this, a clear contrast
difference confirms the formation of a new Fe–Si
phase. It is expected that increasing the sintering
temperature has resulted into more diffusion, result-
ing in intermetallic phase formation and densification.
Micrograph of the nano composite 2SF1200(3) in
Figure 2(d) shows the grains to be uniformly distrib-
uted, which concludes that the silicon is completely
mixed with the iron matrix and thus formed iron–sili-
con phase within the sample. Increasing the sintering
time provides a sufficient duration for diffusion to
occur, which results in better sintering. Therefore, it
is concluded that both the high Si content and lower
sintering temperature have hindered the formation of
intermetallic Fe–Si phase. When the Si content is
decreased from 5% to 2%, a dense and uniform
microstructure is observed after sintering at higher
temperature i.e. 1200(1) and 1200(3).
Energy-dispersive spectroscopy
Figure 3 shows the EDX analysis of the specimens
5SF1000(3), 2SF1100(3), 2SF1200(1), and 2SF1
200(3) for elemental analysis. It is observed that in
spectrum 2 and 3, there is presence of oxygen and
iron within the sample, this indicates that entrapment
of oxygen during the sintering process has taken place
within the sample. This is also in confirmation with
phase analysis shown in Figure 1(a). Apart from this,
there is also a formation of iron oxide in the sample.
In spectrum 4, the iron is present as the main constitu-
ent within the matrix. In spectrum 5, the overall per-
centage of silicon is 3.09% by weight, this indicates
that the addition of the silicon should be lower than
3%, as excessive silicon did not form bond with iron
matrix. Therefore, the samples prepared after this are
having silicon content of 2% in the iron matrix. EDX
results of 2SF1100(3) are shown in Figure 4. In the
spectrum 2 and 3, we can see only small amount of
trapped oxygen and overall distribution of the silicon
Saxena et al.
Figure 3. EDX of 5SF1000(3).
in the sample. In spectrum 5, the overall silicon per-
centage is found to be 3.46, which indicates that max-
imum amount of silicon forms a bond with iron
matrix. Figure 5 shows the EDX results of
2SF1200(1). In the spectrum 2, 3, and 4, silicon is
non-homogenously distributed as it has a little vari-
ation in the amount. In the spectrum 2, more dark
region illustrates more percentage of iron. In spec-
trum 4, the overall composition of silicon is 3.46 by
weight percentage. In Figure 6, EDX results of
2SF1200(3) are shown. In the spectrum 1 and 3, we
can see that only iron is present within the spectrum.
The excessive amount of silicon at spectrum 2 and
overall silicon percentage 1.22 are observed in spec-
trum 5, which indicates that nearly all the silicon
bonds with iron matrix. Percentage of silicon varies
which gives an indication that the silicon is not homo-
genously distributed throughout the sample.
Density and hardness
Green and sintered density, measured for each speci-
men, is listed in Table 3. It is clear from the obtained
values that there is a decrease in the density of speci-
men 5SF1000(3) after sintering. It indicates that the
addition of a higher content of Si (i.e. 5%) causes a
lack in the bonding between Fe and Si during sinter-
ing. This leads to the cracks in specimen and hence the
density has decreased. Measured Rockwell hardness
5
of the same specimen is 37 HRH. For specimen
2SF1100(3), it is observed that there is an increase
in the density after sintering at 1100  C for 3 h. It con-
firms the proper sintering and bonding between Fe
and Si atoms. Further, all the composites containing
2% Si have shown an increased density after sintering
at different temperature schedules. For specimens
2SF1100(3), the measured hardness is 25 HRH.
Sintered density of specimen 2SF1200(1) is higher
than that of the green density. This indicates that
the specimen becomes densified after sintering.
Sintered density of the specimen is however less
than that of sample 2SF1100(3), but the hardness
value significantly increases up to 44 HRH, hence as
the sintering temperature increases the value of hard-
ness increases significantly. In the sample 2SF1200(3),
the sintered density is higher than that of green dens-
ity, this indicates better consolidation and densifica-
tion of the sample. Density of the sample was higher
than that of 2SF1200(1), which indicates that increas-
ing the sintering time leads to better sintering, hence
densification has taken place. Hardness of the sample
2SF1200(3) is found out to be 38 HRH. In case of
metals, solid-state sintering results in densification.
During solid-state-sintering, diffusion between differ-
ent metals results in the neck formation and their
growth.17,18 In the present work, diffusion between
Fe and Si has resulted in Fe–Si phase formation,
which helped in the densification of prepared
6 Proc IMechE Part L: J Materials: Design and Applications 0(0)

Figure 4. EDX of 2SF1100(3).

Figure 5. EDX of 2SF1200(1).

Saxena et al. 7

Figure 6. EDX of 2SF1200(3).

Table 3. Density and hardness of Fe–Si specimens. Table 4. Wear rate of Fe–Si specimens.

Rockwell Wear rate Wear rate Wear rate Wear rate

Green Sintered hardness S. Specimen (mm3/km) (mm3/km) (mm3/km) (mm3/km)
S. No. Samples density density (HRH) No. code 0.5 kg 1 kg 1.5 kg 2 kg

1 5SF1000(3) 4.965 g/cc 4.835 g/cc 37 HRH 1 5SF1000(3) 0.4340 0.5437 2.597 –
2 2SF1100(3) 5.438 g/cc 5.766 g/cc 25 HRH 2 2SF1100(3) 0.6574 0.8744 2.086 –
3 2SF1200(1) 5.291 g/cc 5.530 g/cc 44 HRH 3 2SF1200(1) 0.3529 0.3705 0.4458 0.6024
4 2SF1200(3) 5.251 g/cc 5.550 g/cc 38 HRH 4 2SF1200(3) 0.2797 0.3435 0.4243 0.5986

specimens. Upto 2% Si content and higher sintering

temperature, the bonding between both the metals is
better but at higher Si content i.e. 5%, the brittle
behavior is observed which is due to insufficient
bonding.
Wear rate
Wear rate calculated for prepared Fe–Si specimens is
given in Table 4. Wear rate of specimen is calculated
on the basis of total volume loss occurred during the
experiment. Table 4 shows the wear rate of different
specimens performed at 0.5, 1.0, 1.5, and 2 kg, respect-
ively. For specimen 5SF1000(3), a less wear loss at
low load condition is observed as compared to the
2SF1100(3). But, at high load condition i.e. 1.5 kg,
the wear rate increases significantly. In case of
2SF1200(1), wear rate significantly decreases than
both 5SF1000(3) and 2SF1100(3) specimen. This is
due to the increase in improved sintering mechanism
within the sample which leads to the increased hard-
ness of sample. Therefore, wear rate decreases than
the 5SF1000(3) and 2SF1100(3) specimens. A lower
wear rate of 2SF1200(3) is observed than that of
2SF1200(1), this happens due to solid-state sintering
because of increased sintering time, which leads to
more densified structure and strongly bounded
grains. The strongly bonded structure reduces the
wear rate of the specimen.
8 Proc IMechE Part L: J Materials: Design and Applications 0(0)

SEM of (Fe–Si) worn surface. Figure 7 (a) and (b) shows

the microstructures of the 2SF1200(1) worn surfaces
at 0.5 and 2.0 kg, and 7(c) and (d) shows the micro-
structures of the 2SF1200(3) worn surfaces at 0.5 and
2.0 kg, respectively, captured at 500 magnification.
In case of 2SF1200(1), micrograph of the specimens
tested at 2 kg load shows more material loss than the
loss observed at 0.5 kg load. The grain particles
of iron and silicon are visible. Adhesive wear mech-
anism is prominent at 0.5 kg load condition where
the particles removed due to abrasion get attached
to the disc. At 2 kg load, abrasive wear with micro
ploughing is observed from the micrographs. Micro
ploughing has resulted due to the increased friction
between sample surface and disc at higher load con-
ditions.19,20 In case of 2SF1200(3), wear rate is
reduced due to the homogenous distribution of iron
and silicon where no separation of grains is observed.
Fe–Si particles formed during sintering rub out of the
surface and results in abrasive wear at higher load
conditions.
Characterization of Fe–Si-reinforced
Al2O3 MMNC
Four different specimens were synthesized by reinfor-
cing Al2O3 in Fe–Si alloy-based matrix. Selected com-
position and sintering parameters are listed in Table 5.
Study of different characterizations such as XRD,
SEM, EDX, density, hardness, and wear analysis
results are discussed below.
X-ray diffraction
XRD patterns of specimens 5A2SF1200(1),
5A2SF1200(3), 10A2SF1200(1), and 10A2SF1200(3)
are shown in Figure 8(a) to (d). Presence of differ-
ent phases is matched with standard JCPDS files.
Figure 8(a) shows the XRD pattern of specimen
5A2SF1200(1). Major peaks of iron are observed in
the diffraction pattern, whereas less intense peaks of
iron aluminate (FeAl2O4) compound is also evident.
Reactive sintering between metal and ceramic reinforced
particles has resulted in the formation of FeAl2O4.
Figure 8(b) shows the XRD pattern of
5A2SF1200(3). A major peak of iron along with
iron aluminum oxide is observed in the pattern.
Formation of oxides such as iron oxide (Fe2O3), sili-
con oxide (SiO2), and iron silicon oxide (FeSiO3) is
also formed which indicates that increase in sintering
time promotes the oxidation of free silicon present at
specimen surface.
From Figure 8(c), the major peaks of Fe and
FeAl2O4 are observed in XRD pattern of the specimen
10A2SF1200(1). XRD pattern of specimen
10A2SF1200(3) is shown in Figure 8(d). Along with
the major Fe peaks, a few less intense peaks of new
iron phase (FeAl2O4) and silica (SiO2) are also observed.
Some amount of silicon and aluminum oxide is also left
unreacted within the sample. It is concluded from the
XRD patterns of Al2O3-reinforced Fe–Si-based
MMNCs that the reinforcement amount, sintering tem-
perature, and sintering time affect the phase evolution
and resulting properties. Increasing the reinforcement

Figure 7. Worn surface analysis of (a) 2SF1200(1) at 0.5 kg and (b) 2.0 kg, respectively, and 2SF1200(3) at (c) 0.5 kg and (d) 2.0 kg,
respectively at 500 magnification.

Table 5. Samples of Fe–Si-reinforced Al2O3 metal matrix nanocomposites (MMNCs).

Composition (wt. %)
Sintering
Sample No. Iron (%) Silicon (%) Alumina (%) temperature Sintering time Nomenclature

1 93.1 1.9 5 1200  C 1 hours 5A2SF1200(1)

2 93.1 1.9 5 1200  C 3 hours 5A2SF1200(3)
3 88.2 1.8 10 1200  C 1 hours 10A2SF1200(1)
4 88.2 1.8 10 1200  C 3 hours 10A2SF1200(3)
Saxena et al.
Figure 8. XRD of (a) 5A2SF1200(1), (b) 5A2SF1200(3) (c) 10A2SF1200(1), and (d) 10A2SF1200(3).
Figure 9. SEM of (a) 5A2SF1200(1), (b) 5A2SF1200(3), (c) 10A2SF1200(1), and (d) 10A2SF1200(3) at 500 magnification.
content increases the intensity of intermediate com-
pound such as FeAl2O4 and Al2O3. When the sintering
time increases, it helps in increasing the reactive sinter-
ing between metal matrix and reinforcement phase.
Increasing the sintering time enhances this phenom-
enon. This is the reason of maximum FeAl2O4 forma-
tion in 10A2SF1200(3) specimen.
Scanning electron microscopy
Figure 9(a) to (d) shows the the SEM images of spe-
cimens 5A2SF1200(1), 5A2SF1200(3), 10A2SF12
00(1), and 10A2SF1200(3), respectively at 500 mag-
nification. Densification and phase distribution can be
visualized from the above micrographs.
Figure 9(a) shows the uniform distribution of
reinforcement phase in Fe–Si alloy matrix and
9
presence of few pores in 5A2SF1200(1) microstruc-
ture. FeAl2O4 phase formation is occurred as a
result of reactive sintering between Fe and Al2O3 par-
ticles. From Figure 9(b), a well-dense microstructure
with uniformly distributed grain boundaries can be
observed in the micrograph. There is absence of any
unreacted particle on the surface, which indicates the
complete diffusion of metals and reactive sintering
between metal and ceramic phases.21 Figure 9(c)
shows a contrast difference in the micrographs
which indicate the formation of a new phase in
10A2SF1200(1). Along with this, the densified surface
can be seen where the reinforcement phase is depos-
ited at the grain boundaries. There is no unreacted
particle of silicon and alumina present which indicates
the complete diffusion and reactive sintering mechan-
ism. In Figure 9(d), microstructure shows the
10 Proc IMechE Part L: J Materials: Design and Applications 0(0)

Figure 10. EDX of 5A2SF1200(1).

Figure 11. EDX of 5A2SF1200(3).

Saxena et al.
uniformity of the material but pores are present in the
material. White spots shown in the micrograph are of
alumina. It indicates that some alumina has not
involved in reactive sintering and remains unreacted
which has contributed in the formation of pores and
cracks on the specimen surface.
Energy-dispersive spectroscopy
EDX of specimens 5A2SF1200(1), 5A2SF1200(3),
10A2SF1200(1), and 10A2SF1200(3) is performed
for the elemental analysis. In Figure 10, the EDX
results of sample 5A2SF1200(1) are shown where
four different regions have been captured for analysis.
In spectrum 2, the iron is present as the main constitu-
ent within the matrix as 97.79% by weight and silicon
is about 0.14%. Alumina percentage is significantly
less i.e. 1.96% by weight. In spectrum 3, there is a
presence of oxygen and aluminum which is 48.73
and 26.88 respectively, the iron percentage by weight
is considerably less i.e. 18.25%. Spectrum 1 indicates
the entrapment of oxygen during the sintering
process which is 41.21% and aluminium as 24.62%.
Percentage of iron in the matrix is very less
i.e. 23.02% by weight. In spectrum 4, there is
42.90% of iron and 6% of silicon with aluminium
as 29.07%.
Figure 12. EDX of 10A2SF1200(1).
11
From Figure 11, the EDX results of 5A2SF1200(3)
indicate the formation of Fe–Si within the sample
with 66.89% iron and silicon as 33.11% silicon con-
tent. Spectrum 5 shows the variation within the
materials homogeniously throughout as 70.98%
iron, 5.48% silicon, and 8.11% of aluminium
throughout the sample. In spectrum 2 and 3, silicon
composition is much higher i.e. 14.74% and 9.79%,
this indicates that the silicon gets dissolved in higher
composition within some area of the matrix. In Figure
12, EDX results of 10A2SF1200(1) are shown.
Spectrum 4 shows little variation in silicon and alu-
minium throughout the sample. In spectrum 2 and 3,
formation of iron aluminate phase is confirmed.
Figure 13 shows the EDX results of 10A2SF1200(3).
Spectrum 3 is a pure iron phase. In spectrum 4, silicon
and alumina are homogenously distributed through-
out having a little variation in the amount. Spectrum
2 and 3 have high percentage of silicon within the
matrix.
Density and hardness
Green and sintered density of alumina-reinforced
5A2SF1200(1), 5A2SF1200(3), 10A2SF1200(1), and
10A2SF1200(3) MMNCs is listed in Table 6. A reduc-
tion in the density values is observed after addition of
12 Proc IMechE Part L: J Materials: Design and Applications 0(0)

Figure 13. EDX of 10A2SF1200(3).

Al2O3 particles. Densification has occurred due to Table 6. Density and hardness of Al2O3-reinforced Fe-Si
solid-state sintering process. Sintered density of speci- metal matrix nanocomposites (MMNCs).
mens 5A2SF1200(1) and 5A2SF1200(3) is 5.139 g/cc
Rockwell
and 5.208 g/cc, respectively. Specimen 5A2SF1200(3) Green Sintered hardness
becomes more dense than 5A2SF1200(1) this is S. No. Samples density density (HRH)
because increasing the sintering time leads to increase
in the solid-state sintering process. Sintered density of 1 5A2SF1200(1) 4.886 g/cc 5.139 g/cc 46
10A2SF1200(1) and 10A2SF1200(3) is 4.58 g/cc and 2 5A2SF1200(3) 4.906 g/cc 5.208 g/cc 62
4.56 g/cc, respectively. There is a decrease in density 3 10A2SF1200(1) 4.428 g/cc 4.580 g/cc 55
values with increasing Al2O3 content. This decrease is 4 10A2SF1200(3) 4.449 g/cc 4.563 g/cc 36
observed due to the lesser theoretical density of alu-
mina as compared to iron and silicon. Highest density
is observed for 5A2SF1200(3) specimen, when com- 36 HRH, respectively. Increasing the Al2O3 content
pared to other specimens which indicate a better from 5% to 10% reduces the hardness due to insuffi-
sintering in 5A2SF1200(3) as compared to other cient bonding between alloy matrix and ceramic
specimens. reinforcement. At higher reinforcement content, cer-
Table 6 also shows the hardness values of prepared amic to ceramic particle contact has increased and
composites. Hardness values observed for specimens matrix is not able to surround them properly.
5A2SF1200(1) and 5A2SF1200(3) are found out to be Therefore, the particles are not able to withstand
46 HRH and 62 HRH respectively. Presence of Al2O3 against indentation and therefore hardness reduces
particles has hindered the plastic deformation during slightly. Formation of FeAl2O4 compound results
indentation and hence hardness values increases. from reactive sintering which is responsible for
This indicates the reactive sintering between metal improved hardness. When sintering is done for 3 h,
and ceramic particles. When sintering time is more the reactive sintering leads to the formation of more
i.e. 3 h, better bonding between grains has occurred. oxides such as silicon dioxide and aluminum dioxide,
Hardness of specimens 10A2SF1200(1) and which leads to decrease in the formation of FeAl2O4;
10A2SF1200(3) was found out to be 55 HRH and therefore, the hardness value of the samples decreases.
Saxena et al.
Wear rate
Wear rate of Al2O3-reinforced Fe–Si MMNCs, at dif-
ferent load conditions, is listed in Table 7. Sample
5A2SF1200(3) has shown less wear rate at low load con-
dition when compared to the specimens 5A2SF1200(1)
and 10A2SF1200(1). This is due to the more hardness of
5A2SF1200(3) than other specimens. At high load con-
dition i.e. 2 kg, wear rate increases significantly. In spe-
cimen 10A2SF1200(1), more wear rate as compared to
previous two specimens is observed at 0.5 kg. This is due
to the decrease in solid-state sintering at high reinforce-
ment content. The wear rate increases rapidly at 2 kg
load due to the abrasive wear mechanism with its
own debris. When the test was conducted on
specimen 10A2SF1200(3), failure in the specimen has
occurred.
Therefore, it can be concluded that the high sintering
temperature helps in the better diffusion between metal/
metal particles and reactive sintering between metal/cer-
amic particles. But, when the concentration of ceramic
particles is very high (10 wt% in present case), the metal
matrix is not able to surround the ceramic particles and
thus ceramic/ceramic contact increases. This increases
the concentration of defects and results in brittle behav-
ior which causes low density, hardness, and failure in the
material at high load conditions.
SEM of worn surface of Al2O3-reinforced Fe–Si
MMNCs. Micrograph of specimen surface of
5A2SF1200(1), worn at 0.5 and 2.0 kg load, is shown in
Figure 14(a) and (b), respectively at 500  magnification.
High material loss and micro ploughing are observed at
2 kg load for the specimen. Micro ploughing is a process
Table 7. Wear rate of Al2O3-reinforced Fe–Si metal matrix nanocomposites (MMNCs).
Wear rate
(mm3/km)
S. No. Specimen code 0.5 kg
1 5A2SF1200(1) 0.1548
2 5A2SF1200(3) 0.0710
3 10A2SF1200(1) 0.3682
Figure 14. Worn surface analysis of 5A2SF1200(1) at (a) 0.5 kg and (b) 2.0 kg, respectively, and 5A2SF1200(3) at (c) 0.5 kg and
(d) 2.0 kg, respectively at 500  magnification.
13
of material loss which occurs when the debris particles
come in between disc and sample surface during test.
Grains of iron, silicon, and alumina can be observed
clearly coming out of the surface.
In Figure 14(c) and (d), the micrograph of worn
sample 5A2SF1200(3) is shown, tested under load of
0.5 and 2.0 kg, respectively at 500  magnification. At
0.5 kg load, the micrograph shows wear loss due to
adhesive wear therefore the wear rate is significantly
very less and worn marks are slight. This reduced
wear rate is due to the presence of hard iron aluminate
phase resulting from the reactive sintering between alloy
matrix and reinforced phases. It holds the alloy matrix
during sliding and reduces the material removal.
Micrograph of worn surface examined at 2 kg load
shows higher wear rate as well as higher micro plough-
ing rate than that of 0.5 kg load. This increase in the
wear rate is due to the increase in load thus more par-
ticles are worn out. This causes the debris particles to
adhere on the disc which leads to the increase in wear
loss. But unlike other sample 5A2SF1200(1), at higher
load, no definite loose particles are seen at 2000, this
indicates that all the grains are bonded tightly to each
other and are thus resisting material loss.
Conclusion
The present work reports phase, microstructure, and
wear behavior of Al2O3-reinforced Fe–Si alloy-based
MMNCs processed via P/M technique. There are fol-
lowing outcomes of the current study.
1. Amount of Si in matrix phase, ceramic reinforce-
ment (Al2O3) content, and sintering schedule has
Wear rate Wear rate Wear rate
(mm3/km) (mm3/km) (mm3/km)
1 kg 1.5 kg 2 kg
0.1868 0.1990 0.2789
0.1058 0.4324 0.7077
1.3751 21.1410 25.8422
14
affected the phase formation, microstructure, and
mechanical behavior of prepared composites.
2. High content of Si in alloy composition resulted in
the lack of bonding which leads in the free Si and
its oxide formation. A lack in density, hardness,
and wear resistance is observed at 5 wt.% Si con-
tent. Up to 2 wt.% Si, complete Fe–Si alloy for-
mation, better density, and mechanical behavior is
observed. Intermetallic Fe–Si phase has formed as
a result of diffusion between Fe and Si elements.
Along with this, increasing the sintering tempera-
ture and time resulted in more diffusion, Fe–Si
phase formation, and better mechanical behavior.
3. Addition of ceramic Al2O3 particles provided sup-
port to the matrix phase by hindering the plastic
deformation, when external force is applied. Upto
5 wt.% Al2O3 reinforcement, the improvement in
mechanical behavior is observed but property deg-
radation has started at 10 wt.% Al2O3 content. This
change in behavior is due to the insufficient coating of
ceramic particles by matrix phase thus leading to high
ceramic–ceramic contact. Formation of FeAl2O4
intermediate compound has formed as a result of
reactive sintering between metal matrix and ceramic
particles. Maximum phase formation is achieved for
specimens sintered at 1200  C for 3 h. This new phase
is found responsible for the improved mechanical
behavior of prepared nano composites.
Declaration of conflicting interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of
this article.
Funding
The author(s) received no financial support for the research,
authorship, and/or publication of this article.
ORCID iD
Pallav Gupta https://orcid.org/0000-0002-3218-1200
References
1. Ponnamma D, Sadasivuni KK, Grohens Y, et al. Carbon
nanotube based elastomer composites—an approach
towards multifunctional materials. J Mater Chem C
2014; 2: 8446–8485.
2. Sadasivuni KK, Ponnamma D, UKo H, et al. Flexible NO2
sensors from renewable cellulose nanocrystals/iron oxide
composites. Sensor Actuat B-Chem 2016; 233: 633–638.
3. Gupta P, Kumar D, Parkash O, et al. Sintering and
hardness behavior of Fe-Al2O3 metal matrix nanocom-
posites (MMNCs) prepared by powder metallurgy. J
Compos 2014; 145973: 1–10.
4. Tjong SC and Lau KC. Microstructural and mechanical
characteristics of in situ metal matrix composites. Mater
Lett 2000; 43: 274–280.
5. Kumar UJP, Gupta P, Jha AK, et al. Closed die deform-
ation behavior of cylindrical iron-alumina metal matrix
Proc IMechE Part L: J Materials: Design and Applications 0(0)
composites during cold sinter forging. J Inst Eng India
Ser D 2016; 97: 135–151.
6. Singh N, Banerjee S, Parkash O, et al. Structural and mech-
anical behaviour of Fe-30Ni alloy produced by a powder
metallurgy route. Trans Ind Ceram Soc 2017; 76: 38–42.
7. Soltani N, Pech-Canul MI and Bahrami A. Effect of
10Ce-TZP/Al2O3 nanocomposite particle amount and
sintering temperature on the microstructure and mech-
anical properties of Al/(10Ce-TZP/Al2O3) nanocompo-
sites. Mater Design 2013; 50: 85–91.
8. Fayyad EM, Sadasivuni KK, Ponnamma D, et al. Oleic
acid-grafted chitosan/graphene oxide composite coating
for corrosion protection of carbon steel. Carbohydr
Polym 2016; 151: 871–878.
9. Soltani N, Sadrnezhaad SK and Bahrami A.
Manufacturing wear-resistant 10Ce-TZP/Al2O3 nano-
particle aluminum composite by powder metallurgy
processing. Mater Manuf Process 2014; 29: 1237–1244.
10. Gupta P, Kumar D, Parkash O, et al. Structural and
mechanical behavior of 5% Al2O3 reinforced Fe metal
matrix composites (MMC) produced by powder metal-
lurgy (P/M) route. B Mater Sci 2013; 36: 859–868.
11. Gupta P, Kumar D, Parkash O, et al. Hardness and
wear behavior of CoO doped Fe-Al2O3 metal matrix
composite (MMC) synthesized via powder metallurgy
(P/M) technique. Adv Mat Res 2012; 585: 584–589.
12. Jha P, Gupta P, Kumar D, et al. Synthesis and charac-
terization of Fe–ZrO2 metal matrix composites.
J Compos Mater 2014; 48: 2107–2115.
13. Gupta P, Kumar D, Parkash O, et al. Effect of sintering
on wear characteristics of Fe-Al2O3 metal matrix com-
posites. P I Mech Eng J-J Eng 2014; 228: 362–368.
14. Singh N, Banerjee S, Parkash O, et al. Tribological and
corrosion behavior of (100-x)(Fe70Ni30)-(x)ZrO2 com-
posites synthesized by powder metallurgy. Mater
Chem Phys 2018; 205: 261–268.
15. Gupta P, Kumar D, Quraishi MA, et al. Effect of cobalt
oxide doping on the corrosion behavior of iron-alumina
metal matrix nanocomposites. Adv Sci Eng Med 2013;
5: 1279–1291.
16. Hussain Z, Chew GT and Projjal B. Microstructure and
hardness characterization of mechanically alloyed Fe-C
elemental powder mixture. Mater Design 2010; 31:
2211–2215.
17. Slipenyuk A, Kuprin V, Milman Yu, et al. Properties of
P/M processed particle reinforced metal matrix com-
posites specified by reinforcement concentration and
matrix-to-reinforcement particle size ratio. Acta Mater
2006; 54: 157–166.
18. Singh N, Parkash O and Kumar D. Phase evolution,
mechanical and corrosion behavior of Fe(100-x)Ni(x)
alloys synthesized by powder metallurgy. J Phys Chem
Solids 2018; 114: 8–20.
19. Gupta P, Kumar D, Parkash O, et al. Dependence of
wear behavior on sintering mechanism for iron-alumina
metal matrix nanocomposites. Mater Chem Phys 2018;
220: 441–448.
20. Mehta J, Mittal VK and Gupta P. Role of thermal
spray coatings on wear, erosion and corrosion behavior:
a review. J App Sci Eng 2017; 20: 445–452.
21. Garg P, Jamwal A, Kumar D, et al. Advance research
progresses in aluminium matrix composites: manufactur-
ing & applications. J Mater Res Tech 2019; 8: 4924–4939.