Accepted Manuscript

Vanadium carbide reinforced aluminum matrix composite prepared by conventional,

microwave and spark plasma sintering

Ehsan Ghasali, Amir Hossein Pakseresht, Masoud Alizadeh, Kamyar

Shirvanimoghaddam, Touradj Ebadzadeh

PII: S0925-8388(16)32096-5
DOI: 10.1016/j.jallcom.2016.07.063
Reference: JALCOM 38231

To appear in: Journal of Alloys and Compounds

Received Date: 6 June 2016

Revised Date: 2 July 2016
Accepted Date: 5 July 2016

Please cite this article as: E. Ghasali, A.H. Pakseresht, M. Alizadeh, K. Shirvanimoghaddam, T.
Ebadzadeh, Vanadium carbide reinforced aluminum matrix composite prepared by conventional,
microwave and spark plasma sintering, Journal of Alloys and Compounds (2016), doi: 10.1016/
j.jallcom.2016.07.063.

This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to
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 ACCEPTED MANUSCRIPT

Vanadium carbide reinforced aluminum matrix composite prepared by

conventional, microwave and spark plasma sintering
Ehsan Ghasali a,*, Amir Hossein Pakseresht a, Masoud Alizadeh a, Kamyar Shirvanimoghaddam
b
,Touradj Ebadzadeh a
a
Ceramic Dept, Materials and Energy Research Center, Alborz, Iran

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b
Institute for Frontier Materials, Deakin University, Waurn Ponds, Geelong, Victoria 3216, Australia

*Corresponding author: Tel : 0098 26 36280040; fax: 0098 26 36201888.

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E-mail address: Ehsan_ghasali@yahoo.com

Abstract

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The effect of sintering method on the structure and mechanical properties of aluminum -10 wt%
VC composite was investigated. Aluminum-VC metal matrix composite was prepared

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successfully by conventional (at 600°C), microwave (at 600°C) and spark plasma sintering (at
450°C). The obtained results indicate that the aluminum -10 wt% VC composite prepared by
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SPS had the highest relative density (99±0.6±%TD), bending strength (295±15 MPa) and
microhardness (232±16 Vickers). The XRD investigations showed the decomposition of VC
phase and the formation of Al3V intermetallic phase in the microwave-sintered samples. The
SEM micrographs and EDS analyses revealed uniform distribution of reinforcement particles in
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SPS method and the formation of Al3V phase in microwave-sintered sample.

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Keyword: Aluminum, Vanadium carbide, Microwave, Spark Plasma Sintering.

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1. Introduction

In the past few decades, aluminum matrix composites (AMCs) have been considered in
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aerospace projects, auto motive and military industries due to significant properties such as high
specific strength, modules and toughness [1-4]. Particulate reinforcements which were used in
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aluminum (Al) composite significantly improved the properties of AMCs due to their high
hardness and strength combined with ductile aluminum matrix [5-8]. Many factors such as
uniform distribution of reinforcements, thermal expansion difference, production conditions and
etc. that affect the mechanical properties have been investigated by numerous researchers. But
the chemical compatibility between reinforcement and matrix is the most important of above-
mentioned factors [9-11]. It is worth to mention that this compatibility has a complicated
influence on the final properties. Some researchers believe that the reaction between
reinforcement and matrix has destructive effect on the final properties [12, 13], while others have

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introduced the amounts and quality of products formed in the results of interfacial reaction
between reinforcements and matrix [14, 15].
Ceramic particulate reinforcements help to improve the soft aluminum matrix in terms of
hardness, strength and wear resistance. The improvement depends on the amount and uniformity
of distribution of reinforcements, and the strength of the particle-matrix boundary and the
mechanical properties of the matrix [16].

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Transition metal carbides such as HfC, TiC, VC, TaC are commercially important because of
their extreme hardness and also their application in wear resistant parts [17]. Their excellent
high-temperature strength and good corrosion resistance make them useful as high-temperature

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structural materials [18]. Many binary metal carbides have shown high microhardness values
which make them them as suitable candidates for reinforcement particles in aluminum matrix
composites [19].

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Transition-metal aluminides such as Al3Ti, Al3V, Al3Nb and etc. are among the most promising
candidates for high-performance structural materials due to their high mechanical properties
[20]. The intermetallic compounds of Al-Ti, Al-Ta, Al-Nb, Al-V and Al-Mo in Al matrix can

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reduce the difference between thermal expansion coefficient of reinforcements and matrix [21,
22]. Formation of Al3V phase as a result of the reaction between aluminum and vanadium
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carbide has been reported by L. E. Bodrova et al [23]. M. Jahnátek et al [24] showed that the
calculated tensile strength of Al3V with FCC crystal structure is higher than that of Al and V
crystals. Abdel-Nasser [22] reported the formation of Al3V as insitu reinforcement from the
reaction between molten aluminum and V2O5 particles.
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Novel sintering methods such as microwave-assisted hot press, spark plasma sintering, hot
isostatic press and etc introduce specific features for prepared specimens. Reducing sintering
temperature due to the application of pressure in pressure-assisted sintering methods can offer
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better mechanical properties compared to the conventional sintering [25-27].

According to the author’s knowledge, there has never been any research on microwave and spark
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plasma sintering of Al-VC metal matrix composites. In the present work, Al-VC composites
were fabricated successfully by spark plasma, microwave and conventional sintering methods.
Furthermore, the effects of different sintering methods on physical properties, microstructure,
hardness, and bending strength of Al-VC composites were investigated.
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2. Experimental procedures
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2.1. Preparation of composite

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Aluminum (MERCK Art. no. 1056 aluminum powder, 250 mesh 99% purity) and vanadium
carbide (average particle size of 200 nm, 99% purity) powders were used as starting materials.
10 wt% VC was blended with aluminum powder in ethanol media using a high-energy ball mill
and the mixture was dried at 70°C. The bar shape samples with 5×5×25 mm dimensions were
prepared by uniaxial pressing at 250 MPa for conventional and microwave sintering. The mixed
powders were directly used in SPS method without pre-pressing process. Conventional sintering
was done at temperature of 600°C with 10°C/min heating rate in a graphite bed for 1 h.
Microwave sintering was performed in an assembled microwave furnace (900 W and 2.45 GHz)
at 600°C. The mixed powders were directly inserted into a graphite die (30 mm diameter) of a

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SPS ((SPS-20T-10, China) and the sintering process was done at 450°C with initial and final
pressure of 10 MPa (with increasing temperature) and 30 MPa (at temperature of 400°C),
respectively. The phase identification was carried out using XRD (Philips X’ Pert System) with a
Co kα (λ= 1.789 A°) radiation source and an image-plate detector over the 2θ range 5-100° in
reflection geometry. The bulk density of sintered samples was measured using the Archimedes’
principle. The three-point bending flexural test was used to examine the strength of sintered
samples. The bending strength samples fabricated by SPS were cut from sintered disc with 30

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mm diameter. Vickers microhardness values of the sintered samples were calculated using at
least ten successive indentations for each sample by a MKV-h21 Microhardness Tester under a
load of 1kgf for 15 s. Microstructural characterization of sintered samples was examined using

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FESEM (MIRA 3 TESCAN, Czech Republic and S360 Cambridge) equipped with an energy
dispersive spectrometer (EDS). Details of material preparation procedure and sintering process
as well as microstructural investigations are the same as that previously reported [4, 8-11].

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3. Results and discussion

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Fig. 1 shows the variation of sintering temperature versus time for SPS, microwave and
conventional process. As can be seen in Fig. 1, SPS sintering of sample was done at 450°C
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during 9 minutes. The microwave and conventional sintering were performed at 600°C without
soaking time and for 1 h, respectively. The SPS sintering was carried out at higher heating rate
compared to microwave and conventional sintering.
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700

600

500
Temperature (°C)

400

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SPS
300
Microwave

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200

100 Conventional

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0
0 10 20 30 40 50 60 70 80 90 100 110 120 130
Time (min)

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Fig. 1 The variation of temperature vs time for different sintering methods

Fig. 2 reveals x-ray diffraction patterns of sintered samples. For SPS and conventional sintered
samples, the vanadium carbide and aluminum were the only detectable crystalline phases, while
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small peaks of Al3V phase were also detected within microwave sintered sample. The small
peaks of Al3V can be attributed to the low amount of initial VC and also partial decomposition of
VC particles. The presence of aluminides in aluminum powder discussed in the introduction
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section has also been reported by other researchers [9]. For instance, Al3V was found in Al-VC
composite as reported by L. E. Bodrova [23]. The equation 1 shows the Gibbs free energy for
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formation of Al3V [28].

∆G(Al3V) = -26 600 + 8.50273 T (1)

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The formation of Al3V from decomposition of VC and reaction with aluminum at 900°C were
reported by L.E. bodrova [23]. However, they also found Al4C3 and AlV2C compounds
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accompanied by Al3V. Our research shows that the byproducts are not identified due to very
small amounts of probable phases and detection limit of XRD.
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The formation of Al3V in microwave-sintered sample can be explained by the selective

adsorption of microwave irradiation and subsequently selective heating of some materials.
Thermodynamically, Al3V can be formed at temperature of 600°C and handled by the reaction
between aluminum and vanadium carbide. The interfacial reaction continues by diffusion of
elements from aluminum matrix or vice versa. Since carbides have been known to be good
absorbers of microwave radiation because of the strong coupling of carbon with microwaves,
thus VC can produce higher interfacial temperature at the interface of aluminum and VC

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particles. The higher interfacial temperature at some selective areas rather than bulk sample
accelerates the diffusion of elements at those areas and encourages progress in reaction.

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Fig. 2 XRD patterns of Al-10wt%VC composite prepared by spark plasma, microwave and conventional sintering

Fig. 2 also shows the structure of tetragonal Al3V that is in good agreement with XRD card
number 00-065-2664. The Al3V phases with L12 structure are coherent with aluminum matrix
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and therefore they can significantly improve the mechanical strength of alloy. The metal
trialuminides precipitates are quickly transform from the cubic L12 structure to the complex
tetragonal structure (D022) with aging temperature that is higher than a critical temperature [28,
29]. As a result of semi-coherency between D022 and D023 precipitates and aluminum matrix, the
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coherency strengthening of the alloy reduces associated with precipitation at the state of L12
structure [30, 31]. Furthermore, the loss of coherency between the precipitate particles and metal
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matrix accelerates Ostwald ripening of the precipitate particles and consequently, the effect of
precipitation-strengthening of alloy reduces [32, 33].
Fig. 3 and 4 show the punch displacement and displacement rate change with sintering time for
spark plasma sintered sample. In this figure, two important zones are detectable: 1) initial
shrinkage zone between 0 and 4 min sintering time and 2) second, shrinkage zone between 6 and
8 min.
The first shrinkage zone can be related to gas removal and the formation of neck between
particles. The second zone can be considered as sintering process with highest punch
displacement in any stage of sintering process (Fig. 4).

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Investigation of shrinkage during sintering process is very helpful to understand sintering

behavior and these instruments can facilitate choosing appropriate sintering power (including
voltage and amperage) in spark plasma sintering. The important key in SPS method is the
application of appropriate pressure and time at sintering temperature to obtain the maximum
relative density.
72

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Punch displacement(mm)

71.5

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71

70.5

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70

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69.5
0 1 2 3 4 5 6 7 8 9 10
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Time (min)

Fig. 3 The variation of punch displacement with sintering time for SPS sample
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Displacement rate(mm/min)

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0.5
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0
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0 1 2 3 4 5 6 7 8 9 10
Time (min)

Fig. 4 Displacement rate vs sintering time for SPS sample

The pressure during sintering process was started at 10 MPa and increased with increasing
temperature up to 400°C (after 6 min) and reached to 30 MPa to ensure sintering process was
completed with maximum shrinkage. The constant amount of punch displacement after final

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stage of sintering (nearly 7 min) can be related to the end of sintering process with the maximum
relative density.

Fig. 5 demonstrates camera picture of as-received samples after sintering process without any
behind polish operation.

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Fig. 5 Camera picture of as-sintered composites: conventional (a and d), microwave (b and c) and SPS (e).
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Melting areas are not observed in conventional sintered composites (Fig. 5a and d), while the
surface of SPS sintered composite is completely smooth and without melting (Fig. 5e). As can
be seen in Fig. 5b and c, some melting areas are observed in the microwave sintered sample due
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to two possible reasons. The first can be attributed to the existence of Al3V phases accompanied
by liquid phase as the phase diagram of Al-V alloys reveals. The two- phase zone of liquid +
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Al3V will remain at temperatures higher than 703°C [34]. The second can be related to locally
melting of aluminum powders that outgoing with VC particles and subsequently, the reaction
between melted aluminum and VC particles occurs.

Fig. 6 shows SEM micrograph of sample sintered conventionally at 600°C showing some
agglomerates of VC particles and porosities. The agglomeration of VC reinforcements during
sintering process occurs due to low particle size (about 200 nm) which produces a high surface
tension. The formation of agglomerated particles has been reported even with equal amounts of

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other reinforcements such as B4C and ZrB2 in aluminum matrix and nearly the same mixing
process [5, 7]. It seems that a lower particles size of reinforcement and the chemical reaction
between reinforcement and aluminum particles result in the agglomeration of reinforcement
particles; the above-mentioned has been previously reported [35, 36].

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Fig. 6 Backscattered FESEM micrograph of sample sintered conventionally at 600°C

Figs. 7 and 8 demonstrate backscattered FESEM images and EDS analysis of microwave and
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spark plasma sintered samples. Al matrix, VC reinforcements, Al3V phase and porosities are
marked on the microstructure of microwave sintered sample. It seems that besides selective
heating of microwave processing, the formation of Al3V phase led the creation of porosities.
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These porosities can be formed from areas that melting occurs and removes from sample or the
void spaces between agglomerates of VC reinforcements and maybe as consequence of poor
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bonding of Al-Al particles because of initial pores at the first stage of preparation of green
samples before sintering. It seems that the formation of Al3V phases in microwave sintered
samples causes for extraction of unreacted VC particles into the aluminum matrix and
agglomerated area.

Fig. 8 shows different microstructure of spark plasma sintered Al-VC composite. As observed,
Al3V particles were not detected in the microstructure of sintered composite. Low sintering
temperature of 450°C could not cause the reaction between aluminum and VC particles and the
application of pressure has led to a pore-free microstructure.

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Fig. 7 Backscattered FESEM and EDS images of sample sintered by microwave at 600°C

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Fig. 8 Backscattered FESEM and EDS images of sample sintered by SPS at 450°C
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Moreover, in spite of a high difference in thermal expansion coefficient between Al and VC, no
microcracks were found at the interface of Al and VC particles in SPS sintered sample. Also,
uniform distribution of reinforcement particles in Al matrix was observed in the microstructure
of SPS sintered sample which has not been found by other two methods (Figs. 6-8).

Table 1 presents density, bending strength and hardness of prepared composites with different
sintering methods.

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Table. 1 Density, bending strength and microhardness of prepared composites.

Sintering method Density (gr/cm3) Bending strength Microhardness

(MPa) (MPa)

Conventional 2.538±0.01 95±11 88±10

(89±0.3%TD)

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Microwave 2.595±0.01 128±8 102±11
2.823±0.2

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SPS 295±15 232±16
(99±0.6±%TD)
*TD: Theoretical density

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As table 1 reveals a nearly full relative density is obtained for SPS sample. The relative density
of microwave sintered sample could not be calculated from mixture rules due to the formation of
Al3V phases and indistinct amounts of them. The lowest relative density, bending strength and

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microhardness were related to the conventionally sintered sample, while the highest mechanical
properties were measured for SPS samples. S. Nawathe et al [37] reported 47±1 Hv for pure
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aluminum prepared by microwave sintering method. The spark plasma and microwave sintering
of 6061 and 2124 aluminum have been investigated by N. Saheb [38]; increasing temperature
from 400° to 450°C in SPS process led to an increase in the hardness form 56.81 to 66.31 for Al
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6061 alloy. Definitely, aluminum composite reinforced by hard ceramic particles obtains higher
strength and hardness compared to the monolithic aluminum samples. The difference in the
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coefficient of thermal expansion between matrix and reinforcement can produce a high
dislocation density area and also the hard nature of reinforcement particles increases total
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indentation hardness.

As mentioned in the previous section, Al3V phase formed during microwave processing has great
mechanical properties and good bonding to the aluminum matrix. However, the mentioned
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properties are weakened by corporation of porosities in the microstructure. Finally, lower

mechanical properties were obtained for samples sintered in microwave rather than SPS. The
bonding of Al-Al particle cannot complete by microwave or conventional process due to
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pressureless sintering, the formation of oxide layer around aluminum particles and high thermal
expansion mismatch between aluminum and reinforcement particles which lead to make some
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porosities after sintering process as well as the formation of agglomerated particles [40]. The
advantages of spark plasma process such as surface cleaning, rapid heating rate, vacuum
atmosphere and pressure during process can overcome the above mentioned problems and offer
nearly full dense aluminum composite.

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Fig. 9 shows load-extension curves during bending strength test of samples sintered by different
methods. Toughness can be determined by calculating the area under the load-extension bending
curve and it is the energy of mechanical deformation per unit volume prior to fracture. To be
tough, a material should have both high stresses and high strains. Generally, strength indicates
how much force a material can tolerate, while toughness indicates how much energy a material

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can absorb before rupturing [41]. As can be seen in Fig. 9, the maximum area under load
extension correlates to the SPS sample. Considering the fine microstructure, highest relative
density and mechanical properties of SPS samples, it is not unexpected that samples sintered by

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SPS obtain a higher toughness among samples sintered by other methods. Furthermore, the both
large stress and strain can be observed for spark plasma sintered sample (Fig. 9).

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Fig. 9 Load-extension curves during bending strength test for SPS, microwave and conventional sintered samples
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4. Conclusions
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Aluminum-10 wt% VC metal matrix composite was successfully prepared by spark plasma,
microwave and conventional sintering processes. Compared to microwave and conventional
sintering methods, spark plasma sintering had significant enhancement on the microstructure and
mechanical properties of Aluminum-VC composite. The nearly full dense sample with highest
bending strength (295±15 MPa) and microhardness (232±16 Vickers) was obtained by SPS.
Microwave sintering led to the decomposition of VC and formation of Al3V compounds.
However, porosities in the microstructure of composite prepared by microwave heating resulted
in weak mechanical properties.

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High lights

• Al-VC composite was fabricated by using conventional, microwave and spark plasma
sintering.
• Properties of Al-VC composite can be changed by changing sintering methods.
• Microwave sintering leads to formation Al3V compound.
• SPS method has significant effect on the properties of prepared composite.

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