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Original Article

Investigation on microstructural and mechanical

properties of B4 C–aluminum matrix composites
prepared by microwave sintering

Ehsan Ghasali, Masoud Alizadeh ∗ , Touradj Ebadzadeh, Amir hossein Pakseresht,

Ali Rahbari
Ceramic Department, Materials and Energy Research Center, Tehran, Iran

a r t i c l e i n f o a b s t r a c t

Article history: B4 C reinforced aluminum composites were fabricated by microwave heating of the mixture
Received 31 August 2014 of B4 C (10, 15 and 20 wt%) and aluminum powders at 650, 750, 850 and 950 ◦ C. The effect of
Accepted 10 February 2015 different amounts of B4 C on the microstructure and mechanical properties of aluminum
Available online xxx matrix was examined. The maximum bending (238 ± 10 MPa) and compressive strength
(330 ± 10 MPa) values were measured for composites sintered at 950 and 750 ◦ C, respectively.
Keywords: The maximum hardness (112 Vickers) was measured for Al–20 wt% B4 C composite sintered
Aluminum at 850 ◦ C. XRD investigations showed the decomposition of boron carbide and also the for-
Boron carbide mation of Al3 BC by heating the composites at 850 ◦ C. SEM micrographs showed uniform
Microwave sintering distribution of reinforcement particles in Al matrix.
Metal matrix composite © 2015 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier
Editora Ltda. All rights reserved.

extremely hard [6]. Additionally, boron carbide (B4 C) has a high

1. Introduction neutron absorption cross-section making it a valuable mate-
rial for nuclear applications [6]. Despite these advantages, the
Among metal matrix composites, aluminum alloy based com- monolithic B4 C does not seem to be introducing well as an
posites are known as very promising light materials with advanced structural ceramic due to high brittle nature related
enhanced mechanical properties. In fact, by introducing a to shock induction localized at high strain rates [7]. It is known
hard phase either in particulate or fiber form, the modulus that combining the B4 C with a metal can mitigate the prob-
and wear resistance of aluminum alloys could be significantly lems associated with brittleness. By far, the most popular
improved [1–3]. Among different parameters affected by the metal used in joining B4 C for this purpose is aluminum [8–12].
final properties of the composites, the nature of the reinforce- Aluminum wets B4 C well at elevated temperatures. Molten
ment and processing route play a paramount role [4,5]. Boron aluminum has been shown to form a variety of binary and
carbide is an interesting material for many reasons. It has tertiary phases when in contact with B4 C such as Al3 BC, AlB10
low density (2.51 g/cm3 ), excellent chemical resistance and is and Al4 C3 . Among these phases, Al3 BC is the most commonly

∗
Corresponding author.
E-mail: [email protected] (M. Alizadeh).
http://dx.doi.org/10.1016/j.jmrt.2015.02.005
2238-7854/© 2015 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier Editora Ltda. All rights reserved.

Please cite this article in press as: Ghasali E, et al. Investigation on microstructural and mechanical properties of B4 C–aluminum matrix
composites prepared by microwave sintering. J Mater Res Technol. 2015. http://dx.doi.org/10.1016/j.jmrt.2015.02.005
JMRTEC-153; No. of Pages 5
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observed phase [13,14]. The sintering of composite materials

by microwave processing has been known to reduce heating
3. Results and discussion
temperature and time and lead to fine microstructures and
improved mechanical properties [15–22].
3.1. XRD analysis
The boron carbides react strongly with liquid aluminum,
For studying the effect of sintering temperature on the phase
resulting in a variety of compounds, including Al3 BC, AlB24 C4
structure and chemical compound of the composites, four D
(AlB10 ), Al8B4 C7 , Al3 B48 C2 (b-AlB12 ), AlB2 , AlB12 C2 , AlB48 C2 ,
composites (Table 1) were sintered at 650, 750, 850 and 950 ◦ C.
Al4 C3 and a-AlB12.7 [23]. Some studies have reported on
As Fig. 1 shows, the identified phases were Al, B4 C and Al3 BC.
the reactivity of B4 C in aluminum processed by infiltration
It seems that the formation of Al3 BC begins from the temper-
and powder metallurgy techniques and on the formation of
ature of 850 ◦ C [13].
different compounds at different processing temperatures
[24,25,14,26]. The main aims of the present work are the feasi-
bility of the formation of aluminum–B4 C composites by using 3.2. Density
microwave heating and investigation of the mechanical and
structural properties of these composites. As can be seen in Fig. 2, there are no sharp changes in den-
sity of different composites sintered at the same temperature.
Fig. 2 further reveals that composite A with no Co additive
2. Experimental procedures has the minimum density, which implies that Co additive can
act as a binder between Al and B4 C particles. Meanwhile, it
B4 C (Aldrich-378100) and aluminum (1056-merck) powders should be noted that the accurate calculation of relative den-
were used as the starting materials and cobalt powder (99.8% sity of samples is impossible due to partial decomposition of
purity and 5 ␮m mean particle size) was used as an addi- B4 C.
tive. The composition of composite samples is given in
Table 1.
The mixing of powders presented in Table 1 was car-
ried out using the Spex instrument (8000D, Mixer mill). The AI :
mixed powders were compacted to prepare the bar shape AI3BC :
samples with the dimension of 25 mm × 5 mm × 5 mm at B4C :
250 MPa using a uniaxial press. The compression strength
test samples were fabricated using a hydraulic press type 950ºC
to obtain cylindrical preforms with a diameter of 10 mm
and height of 8 mm. The sintering of samples was carried 850ºC
Intensity

out using a microwave furnace (900 W and 2.45 GHz), which

monitored temperature using an optical pyrometer (Model:
RAYR312MSCL2G) at 650 ◦ C, 750 ◦ C, 850 ◦ C and 950 ◦ C without 750ºC
soaking time in a graphite bed. The bulk density of sin-
tered samples was measured using the Archimedes’ Principle.
The three point bending and compressive strength measure-
ments were examined by Santam-STm 20. For bending and
650ºC
compressive strength tests, five and three specimens were
5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80
used, respectively. X-ray diffraction (Philips (30 kV and 25 mA)
diffractometer system with CuK␣ radiation ( = 1.5405 Å)) anal- 2 theta(degree)
yses were performed to identify the phases present in the
Fig. 1 – XRD patterns of composite containing 20 wt% B4 C
Al–B4 C composites. Vickers microhardness values of the sin-
sintered at 650 ◦ C, 750 ◦ C, 850 ◦ C and 950 ◦ C.
tered samples were determined using a Microhardness Tester
(MKV-h21, Akashi) under a load of 1 kgf for 15 s. At least
ten successive indentations were performed for each sample.
Microstructural investigations and EDS analyses of sintered 2.55
samples were carried out using a SEM (Stereoscan 360, Leica
Cambridge). 2.5
Density (gr/Cm3)

2.45

Al-10wt%B4C
2.4
Al-10wt%B4C-1wt%Co
Table 1 – Different compositions of composite samples. Al-15wt%B4C-1.5wt%Co
2.35 Al-20wt%B4C-2wt%Co
Composite Al (wt%) B4 C (wt%) Co (wt%)

A 90 10 0 2.3
600 650 700 750 800 850 900 950 1000
B 89 10 1
C 83.5 15 1.5 Temperature°C
D 78 20 2
Fig. 2 – Density versus sintering temperature.

Please cite this article in press as: Ghasali E, et al. Investigation on microstructural and mechanical properties of B4 C–aluminum matrix
composites prepared by microwave sintering. J Mater Res Technol. 2015. http://dx.doi.org/10.1016/j.jmrt.2015.02.005
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Fig. 3 – Backscattered images of B and C composites sintered at 850 ◦ C: (a) Al–10 wt% B4 C–1 wt% Co and (b) Al–15 wt%
B4 C–1.5 wt% Co.

Fig. 4 – Backscattered images of A and B composites sintered at 750 ◦ C: (a) Al–10 wt% B4 C and (b) Al–10 wt% B4 C–1 wt% Co.

3.3. Microstructural analysis

Mechanical and physical properties are highly affected by the

microstructure of sintered composites. Figs. 3 and 4 illustrate
3
the SEM micrographs of A, B and C composites. Homogeneous
distribution of B4 C reinforcements can be seen typically in 2
Fig. 3. From Fig. 4(a) and (b), it is observed that A composite 1

in contrast to B composite has some porosity around the B4 C

reinforcement particles. It seems that Co additive can improve
the adherence of Al matrix to B4 C particles.
Fig. 5 shows SEM and EDS micrographs of Al–20% B4 C–2%
Co composite sintered at 850 ◦ C. Also, the EDS spectra, from
some spots labeled 1 through 3, are shown in Fig. 5. Since the 10 μm

EDS analysis is incapable of detection of carbon and boron ele-

ments, the detection of Al peaks in the EDS spectra can be used Spot 1 Spot 2
AI
Spot 3
AI
as a criterion for proofing of B4 C existence in the microstruc-
ture. In spot 1, there are not any peaks, while at spot 2, Al
peak is seen, which probably seems that the interfacial reac-
0 Kev 10 0 Kev 10 0 Kev 10
tion and formation of Al3 BC phase have occurred. In spot 3
stronger peak of Al is observed in the matrix of composite.
Fig. 5 – Backscattered image and EDS of Al–20% B4 C–2% Co
Finally, it seems that the dark and light regions are B4 C and
composite sintered at 850 ◦ C.
Al particles, respectively and Al3 BC is probably formed at the
interface of these particles.
√
the Hall–Petch law:  y ∝ 1/ D, where D is the grain size. (2)
3.4. Bending strength Higher dislocation density generated by the CTE mismatch
between matrix and reinforcements. (3) Chemical reaction
The matrix hardening is mainly the consequence of three between the reinforcements particles and Al matrix, as it can
effects: (1) smaller grain sizes in the AMC matrix than in the have a significant effect on the interfacial characteristics and
alloy due to the reinforcement tangle. The hardening follows hence on the mechanical properties of the composite [27,28].

Please cite this article in press as: Ghasali E, et al. Investigation on microstructural and mechanical properties of B4 C–aluminum matrix
composites prepared by microwave sintering. J Mater Res Technol. 2015. http://dx.doi.org/10.1016/j.jmrt.2015.02.005
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250 120

110
Bending strength(MPa)

200

100
150

90

hardness
100
Al-10wt% B4C
80
Al-10wt% B4C-1wt% Co
50 Al-15 wt%B4C-1.5 wt%Co
70
Al-20wt%B4C-2 wt%Co
0 Al-10 wt%B4C
600 650 700 750 800 850 900 950 1000 60
Al-10 wt%B4C-1 wt%Co
Temperature°C
50 Al-15 wt%B4C-1.5 wt%Co
Fig. 6 – A plot showing variation in bending strength of Al-20 wt%B4C-2 wt%Co
40
composites with sintering temperature.
600 650 700 750 800 850 900 950 1000
Temperature°C

The bending strength of B4 C–Al composites fabricated in the Fig. 8 – the effect of sintering temperature on
present work was found to be in the range of 123–238 MPa microhardness on sintered samples.
for B4 C weight percent fractions in the range of 10–20%,
respectively. Fig. 6 illustrates the bending strength changes
of composites versus sintering temperature. As it is clear in The performed studies on the composites fabricated by
Fig. 6, composites have the lowest bending strength among microwave sintering revealed a narrow grain size with uniform
others and Co additive might promote the adhesion of Al to distribution of the reinforcements, and well-bonded inter-
B4 C particles as observed in SEM micrographs (Fig. 4). faces. This may be correlated with the advantage of microwave
The C composites sintered at 650 and 750 ◦ C have higher sintering, which have been proved to produce the composites
bending strength; however, with the raising temperature with small grain size, homogeneous distribution of reinforce-
bending strength of B composites increases (Fig. 6). The inter- ments and proper interfacial characteristic [29,30].
facial reaction and formation of Al3 BC and also more cohesion
between Al matrix and reinforcement as a result of higher 3.6. Microhardness
sintering temperature which causes higher atomic diffusion
could be the possible reason for the above mentioned. It is For all tested samples, the average microhardness of the
obvious that many parameters including interfacial reaction, microwave sintered composites was higher than the cor-
porosity, microcracks, grains size, etc. affect on mechanical responding value for the reference 6061 Al alloy and the
properties of composite; so the evaluation of each individual hardness increased with the increasing amount of B4 C. This
parameter regardless of the impact of others is unreasonable. can be explained by the law of mixtures in the following equa-
tion [19]:
3.5. Compressive strength
Hc = Hm Fm + Hr Fr

The compressive strength results as a function of sintering where Hc , Hm , and Hr are the hardness of the composite,
temperature (Fig. 7) show that an increase in the amount of matrix and reinforcement, respectively, fm and fr are the frac-
B4 C and sintering temperature lead to an increase in the com- tion of matrix and reinforcement, respectively (Fig. 8).
pressive strength. As it was discussed in the bending strength The microhardness increased with increasing reinforce-
section, the smaller grain size will lead to more grain bound- ment, since B4 C is inherently harder than Al matrix and
aries, which can act as strong obstacles to the dislocation the fairly well distribution of the reinforcements improves
motion, leading to the increase of compressive strength. the ability of the soft matrix to resist deformation. Sintering
temperature is another parameter, which influences on the
350 microhardness of the composite. In the Al/B4 C composites,
with raising sintering temperature to 850 ◦ C the microhard-
Compressive strength (MPa)

330
310
ness increased due to decrease in porosity and enhancement
290
of interfacial bonding. At sintering temperature of 950 ◦ C, the
270
250
microhardness of composites decreased probably due to the
Al-10%B4C
230 formation of Al3 BC and the grain coarsening with increasing
210 Al-10%B4C-1%Co sintering temperature.
190 Al-15%B4C-1.5%Co
170 Al-20%B4C-2%Co
150 4. Conclusions
600 650 700 750 800 850 900 950 1000
Temprature°C
Microwave sintering was used successfully to produce Al/B4 C
Fig. 7 – The effect of sintering temperature on compression metal matrix composite. At sintering temperature of 850 ◦ C
strength. and more, the interfacial reaction between Al and B4 C causes

Please cite this article in press as: Ghasali E, et al. Investigation on microstructural and mechanical properties of B4 C–aluminum matrix
composites prepared by microwave sintering. J Mater Res Technol. 2015. http://dx.doi.org/10.1016/j.jmrt.2015.02.005
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Please cite this article in press as: Ghasali E, et al. Investigation on microstructural and mechanical properties of B4 C–aluminum matrix
composites prepared by microwave sintering. J Mater Res Technol. 2015. http://dx.doi.org/10.1016/j.jmrt.2015.02.005