Composites Part B 175 (2019) 107140

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Composites Part B
journal homepage: www.elsevier.com/locate/compositesb

Effect of Al2O3 nanoparticles content and compaction temperature on

properties of Al–Al2O3 coated Cu nanocomposites
W.S. Barakat a, A. Wagih b, Omayma A. Elkady c, A. Abu-Oqail d, A. Fathy b, *, A. EL-Nikhaily a
a
Mechanical Department., Faculty of Industrial Education, Suez Uni., Egypt
b
Department of Mechanical Design and Production Engineering, Faculty of Engineering, Zagazig University, P.O. Box 44519, Egypt
c
Powder Technology Division, Manufacturing Technology Department, Central Metallurgical R & D Institute, P.O. 87, Helwan, 11421, Cairo, Egypt
d
Mechanical Department, Faculty of Industrial Education, Beni-Suef University, Egypt

A R T I C L E I N F O A B S T R A C T

Keywords: This paper presents experimental investigation on the effect of Al2O3 content and compaction temperature on
Al-Al2O3 coated nanocomposites mechanical and wear properties of Al–Al2O3 coated Cu nanocomposites. With the aim of improving wettability
Microhardness and dispersion of high weight fraction of Al2O3 nanoparticles in Al matrix, Al2O3 nanoparticles were electroless
Wear properties
coated by Cu particles. High-energy ball milling followed by hot compaction was applied to manufacture
Electroless deposition
Al–Al2O3 coated Cu nanocomposites. The results showed that increasing Al2O3 nanoparticles content up to 10 wt
% improved hardness and wear properties of samples compacted at 400 ᵒC, while by increasing Al2O3 content to
15 wt%, the properties were negatively affected due to the agglomeration of Al2O3 nanoparticles and the high
reduction of relative density. However, well dispersion of high content of Al2O3, 15 wt%, was achieved in
samples compacted at 700 MPa which improved hardness by 105% compared to pure Al. The hot compaction
temperature highly influenced structural, mechanical and wear properties of compacted samples. Increasing
compaction temperature, reduced crystallite size (49 nm) and increased the relative density of Al–Al2O3 coated
Cu nanocomposites which improved mechanical and wear properties of the produced samples. Applying elec­
troless deposition of Cu over Al2O3 nanoparticles followed by high-energy ball milling and hot compaction at
700 MPa is an efficient procedure for production of Al–Al2O3 coated Cu nanocomposite with relatively high
Al2O3 content.

1. Introduction for production is the inclusion of Al2O3 particle in liquid or semi-liquid

Processing of metal matrix composites (MMCs) usually requires
mixing of soft metal, high ductility, with hard ceramic material, high
strength, to produce a new material with high strength and accepted
ductility. Recently, these MMCs receive not only researchers’ attention
but also designers’ attention due to their applicability in many advanced
applications. For structural applications, aluminum (Al)-based metal
matrix composites have been widely used in aerospace and automotive
industry due to their high stiffness, modulus, specific strength and wear
resistance [1–4].
Alumina (Al2O3) is one of the widely used particles to reinforce Al
matrix due to its availability and excellent material properties such as
high mechanical strength and good chemical stability at elevated tem­
peratures [5]. Different methods have been presented in the literature
for production of A-Al2O3 composites. A simple and economical method
Al and casting [6–9], at which Al2O3 are entrapped between a high
viscous aluminum metal by the application of centrifugal force. Despite,
its low cost, difficulties in achieving homogenous distribution of Al2O3
in Al matrix have been reported especially when Al2O3 particle size
tends to nanosize [10,11]. High-energy ball milling technique has been
reported to achieve the well dispersion of micro-size Al2O3 particles in
Al matrix [12,13]. However, reducing the particle size to nano-size, the
dispersion of reinforcement particles became not an easy task using
conventional mixing due to their large surface-to-volume ratio and lack
of wettability of fine particles in molten Al [14]. To overcome this
problem, several wettability improvement methods have been presented
such as mixing ceramic powders with Mg and Ti powder [15] and
electroless deposition of Ag [16], Ni [17] and Co [18] on the ceramic
nanoparticles. Using these methods, improved strength and wear rates
of the produced nanocomposites were achieved for relatively ceramic

* Corresponding author.
E-mail address: afmeselhy@zu.edu.eg (A. Fathy).

https://doi.org/10.1016/j.compositesb.2019.107140
Received 4 April 2019; Received in revised form 20 June 2019; Accepted 5 July 2019
Available online 9 July 2019
1359-8368/© 2019 Elsevier Ltd. All rights reserved.
W.S. Barakat et al.
small volume fraction [16,17].
Increasing reinforcement volume fraction improves mechanical and
wear properties of the produced nanocomposites [19–21]. However, this
rule of thumb is achievable up to a threshold at which agglomeration
and poor dispersion of ceramic nanoparticles occur [22]. Thus, most of
the available research on metal matrix nanocomposite focusing on small
volume fraction reinforcement. For example, Kang et al. [22] studied the
influence of micro and nano Al2O3 particles addition of the properties of
Al–Al2O3 nanocomposites. Their results show a noticeable improvement
of strength with the addition of Al2O3 nanoparticle with low volume
fraction up to 4%. However, increasing the volume fraction more than
this value, strength reduction occurs due to Al2O3 nanoparticles clus­
tering. This threshold volume fraction can be increased by electroless
deposition of different metals that have better thermal stability and good
wettability with Al such as Cu.
The main objective of this work is to present a novel method for
production of Al–Al2O3 nanocomposite with relatively high-volume
fraction using electroless deposition of Cu nanoparticles over Al2O3,
high energy ball milling and hot compaction. Moreover, the effect of
Al2O3 coated nanoparticles content on the mechanical and wear prop­
erties of the produced nanocomposite is investigated. Additionally, the
influence of hot compaction temperature on the microstructure, me­
chanical and wear properties of the produced nanocomposite and its
effect on the threshold content of Al2O3 coated are investigated.
2. Material and experiments
2.1. Materials preparation
Samples used in this experiment were made of commercial Al pow­
der of 99.99% purity with particle size less than 10 μm (Dop organic
kimya, Ankara, Turkey). Al2O3 powder (M K Impex CORP. Canada.)
with 99.99% purity and 40 nm particle size was used as a reinforcement.
The electroless deposition process is analogous to electroplating with a
slight difference that electroless deposition does not need electrical
currents. In electroless deposition, the electron transferring takes place
through chemical reduction process leading to deposition of metal on
the surface of ceramic by reducing agent. Before the deposition of Cu on
Al2O3, pretreatment of Al2O3 for favorable condition for plating was
applied. The pretreatment of Al2O3 was performed in two steps. The first
step was sensitization of Al2O3 nanoparticles by immersing on 10 wt%
sodium hydroxide solution with magnetic stirring for 1 h, then in
acetone with stirring for 1 h with the aim of cleaning their surface to
eliminate any impurities of ceramic crystals. After that the powders were
filtered and washed by distilled water then dried in electrical furnace at
110 � C for 1 h.
The second step was activation of Al2O3 nanoparticles for surface
metallization. This step is mandatory for such non-conducting materials,
Al2O3 particles, in which the direct deposition of cu is impossible.
Therefore, activation for Al2O3 nanoparticles surfaces was performed by
deposition of silver on their surfaces to facilitate attraction of copper
particles during electroless deposition process. Chemical bath of 3 g/l
silver nitrate and 300 ml formaldehyde was prepared with PH within
range 11–13 was used for deposition of 10 wt% silver on Al2O3 nano­
particles surface. After silver chemical depositions, the solution was
filtrated, washed using distilled water and dried in electrical furnace at
110 � C for 1 h. The electroless deposition of 30 wt% Cu on Al2O3
nanoparticles was performed using chemical path of 35 g/l copper sul­
fate pentahydrate (CuSO4.5H2O), 200 ml/l formaldehyde reducing
agent and 170 g/l Rochelle salt (C4H4O6KNa.4H2O). Rochelle salt was
added to the solution because copper sulfate was not soluble in PH above
4 which increase the complexity of the deposition process. The pH de­
gree of the solution was adjusted greater than 11 using sodium hy­
droxide (NaOH). Then, the solution was filtrated, washed by distilled
water and dried in electrical furnace at 110 � C for 1 h. The coated
nanoparticles were heated up to 500 � C on tube furnace under hydrogen
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Composites Part B 175 (2019) 107140
gas for 2 h to avoid formation of undesired phases.
Mixtures of Al with 5, 10, 15 wt% Al2O3 coated were prepared using
a ball mill machine for 6 h. The ball to powder weight ratio was kept at
1:4. The mixing process was carried out at room temperature and the
rotation speed of the ball mill was kept at 300 rpm. To avoid oxidation of
Al, the mixing vial was filled with argon gas before mixing. After that the
mixed powders were consolidated by hot pressing at two different
temperatures 400 � C and 600 � C with heating rate 10 � C/min under
700 MPa pressure for 45 min dwell time under an argon atmosphere.
The die used for consolidation was stainless steel cylinder with 12 mm
internal diameter.
2.2. Composite characterization
Densification parameters of sintered samples in terms of apparent
porosity and bulk density were measured in an aqueous media by
Archimedes principle, using water as a floating liquid according to JIS
R2205-1992.
The sintered samples were grinded using grit papers with grades 500
up to 2500 and then polishing by 6 μm and 1 μm alumina paste and
etched with Keller’s reagent for microstructural analysis. The micro­
structure of the polished samples was investigated by field emission
scanning electron microscope (FE-SEM).
The phase formation and composition changes during the sintered
process were identified by X-ray diffraction analysis using X-ray
diffractometer with an automated Siemens Model D-5000 diffractom­
eter using Cu K-alpha radiation and operated at 40 KV and 30 mA in the
2θ range of 20� –100� by the step of 0.05� .
The hardness of the consolidated samples was measured by Vickers
microhardness tester at room temperature, on the polished surface. Each
value was an average of at least six randomly hardness indentations by
applying 300 g load with loading time of 15 s.
Dry sliding wear rate of all samples was carried out using a pin-on-
disc at room temperature without lubrication. The pins of 64 mm2 in
contact area for all samples were tested by sliding them on a hardened
steel disc with hardness of 64 HRC and surface roughness of 60 μm under
different loads. The experiments were carried out under four different
normal loads, 5, 10, 15 and 20 N for 1500 rotations, corresponding to a
fixed sliding distance of 471 m, at constant sliding speeds of 1.5 m/s.
During sliding, the wear rate was defined as the weight loss suffered per
unit sliding distance. To compute the wear rate, the wear pin was
cleaned by in acetone and weighed on a microbalance with �0.1 mg
sensitiveness before and after the wear tests. The coefficient of friction
was continuously recorded during wear test by measured the frictional
force using a load cell then divided by the normal load on the specimen.
3. Results
3.1. Microstructure of powder
Fig. 1 shows microstructure of Al2O3 nanoparticles before and after
electroless coating by Cu. As shown in the figure, the microstructure of
the as received powder is almost the same as the powder after coating.
The powders appear after coating with larger dispersion and less
agglomeration which facilitate the dispersion of Al2O3 nanoparticle in Al
matrix during ball milling. Fig. 1(c) shows the EDX analysis of the coated
powder which reflect the presence of Cu, Ag and Al2O3 only without the
accumulation of any other materials during coating process. Fig. 2 shows
XRD analysis of Al2O3 before and after coating with Ag and Cu. The
peaks are shown for only the three phases which also confirm the val­
idity of the electroless coating process for coating Al2O3 nanoparticles
with Cu particles without contamination of other undesired chemicals.
3.2. Microstructure of consolidated samples
Figs. 3 and 4 show microstructures of the consolidated samples at
W.S. Barakat et al.
Fig. 1. Microstructure of Al2O3 nanoparticles (a) before coating, (b) after coating and (c) EDX of powder after coating.
Fig. 2. XRD of Al2O3 nanoparticles after Ag and Cu coating.
two different hot compaction temperatures, 400 ᵒC and 600 ᵒC, respec­
tively. In Fig. 3, micro voids are observed in all the consolidated samples
even in the one that is free of reinforcement (see Fig. 3(a)). Reinforcing
metallic material with ceramics always leads to formation of pores due
to the large difference between surface energy of ceramics and metals
[13,23–25]. Also, the arbitrary shape of ceramic phase influences the
amount of voids in the composite during compaction [26]. Increasing
coated Al2O3 nanoparticles content increases the micro void density in
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Composites Part B 175 (2019) 107140
Fig. 3. SEM micrographs of hot compacted samples at 400 � C: (a) Al, (b) Al–5%
Al2O3, (b) Al–10%Al2O3 and (b) Al–15%Al2O3.
the sample and facilitate the tendency to form macro-sized voids as
shown in Fig. 3(d) for sample contain 15 wt% Al2O3. This due to the
higher compressive strength of Al2O3 coated nanoparticles compared to
Al which makes the required pressure for consolidating Al at 400 ᵒC is
quite low for consolidating Al2O3. In Fig. 4, samples consolidated at 600
ᵒ
C with different Al2O3 coated content, 0, 5, 10 and 15 wt% are shown. It
is observed that the micro-voids are less presented in these samples than
that compacted at 400 ᵒC. The distribution of Al2O3 coated nanoparticles
W.S. Barakat et al. Composites Part B 175 (2019) 107140

is homogeneous in all the samples. To ensure the homogeneity of the

Fig. 4. SEM micrographs of hot compacted samples at 600 � C: (a) Al, (b) Al–5%
Al2O3, (b) Al–10%Al2O3 and (b) Al–15%Al2O3.
consolidated micro-structure, mapping analysis for the sample con­
taining the highest Al2O3 content is shown in Fig. 5. The figure shows the
homogeneous distribution of the constituents without any observation
of agglomeration.
Fig. 6 shows XRD analysis of Al–Al2O3 nanocomposite with different
content of Al2O3 coated Cu nanoparticles compacted at 400 and 600 ᵒC.
The figure confirms the composition of the prepared nanocomposite
without any evidence of precipitation of other undesired chemical
during deposition of Ag and Cu particles. Peak broadening is observed
with increasing Al2O3 content for samples compacted at 400 and 600 ᵒC.
For samples compacted at 400 ᵒC, there is no evidence on reaction be­
tween Cu and Al forming intermetallic phases, while in sample contain
15 wt% Al2O3 and compacted at 600 ᵒC, peaks for intermetallic phase
appear which indicate that reaction occur between Al and Cu. This
intermetallic phase negatively influences the electrical and thermal
properties of the produced nanocomposite [26]. The crystallite size of
the prepared samples with different coated Al2O3 and consolidated at
different temperature is shown in Table 1. It is observed that the crys­
tallite size is reducing with increasing coated Al2O3 content. Addition­
ally, it decreases with increasing the consolidating temperature.

Fig. 5. Mapping of Al–Al2O3 nanocomposite compacted at 600 � C.

4
W.S. Barakat et al. Composites Part B 175 (2019) 107140

Fig. 7. Microhardness of Al–Al2O3 coated Cu nanocomposites consolidated at

two different temperatures: (a) 400 � C and (b) 600 � C.

Fig. 6. XRD analysis of Al–Al2O3 coated Cu nanocomposite consolidated at two

different temperatures: (a) 400 � C and (b) 600 � C.

3.3. Mechanical and wear properties

The microhardness of the Al–Al2O3 coated Cu nanocomposites

consolidated at 400 and 600 ᵒC is shown in Fig. 7. It is observed that
increasing coated Al2O3 nanoparticles content up to 10 wt% improves
microhardness of the consolidated samples at 400 ᵒC. However, the
microhardness is reduced by increasing coated Al2O3 content to 15 wt%.
Unlike, in the samples consolidated at 600 ᵒC, the hardness almost lin­
early increases with increasing coated Al2O3 content.
Fig. 8 shows the wear rate of Al–Al2O3 coated Cu nanocomposites at
different loads, 5, 10, 15 and 20 N and consolidated at different tem­
peratures, 400 and 600 ᵒC. Generally, increasing the applied load in­
creases the wear rate due to the higher penetration of indenter in the
sample which enable higher metal removal rate [27,28]. For samples
consolidated at 400 ᵒC, at the same applied load, the wear rate is reduced
with increasing coated Al2O3 nanoparticles content up to 10 wt%. Fig. 8. Wear rate of Al–Al2O3 coated Cu nanocomposites consolidated at two
However, for larger coated Al2O3 content, the wear rate is increased different temperatures: (a) 400 � C and (b) 600 � C.
again. This is not the case for the samples consolidated at 600 ᵒC at
which the wear rate is reduced with increasing coated Al2O3 content The average coefficient of friction of Al–Al2O3 coated Cu nano­
even for sample contain 15 wt% Al2O3. This observation highlights large composites at different loads, 5, 10, 15 and 20 N and consolidated at two
dependence of wear properties of Al–Al2O3 coated Cu nanocomposites different temperatures, 400 and 600 ᵒC is shown in Fig. 9. The coefficient
on the compaction temperature. of friction is reduced with increasing load due to the higher indentation
depth of the pin in the sample. It is observed that increasing coated
Al2O3 content up to 10 wt% reduces the coefficient of friction of samples
Table 1
compacted at 400 ᵒC. However, increasing coated Al2O3 content to 15 wt
Crystallite size of Al–Al2O3 coated Cu nanocomposites.
% negatively affect the coefficient of friction of the produced composite.
Al2O3% Crystallite size (nm) For samples compacted at 600 ᵒC, the coefficient of friction reduces with
400 � C 600 � C increasing coated Al2O3 due to the presence of Al2O3 hard particles in
0 157.07 290.34
the structure. Again, the compaction temperature influences the prop­
5 143.52 55.90 erties of the manufactured nanocomposites especially at high coated
10 138.63 53.73 Al2O3 content.
15 116.46 49.02 Based on the obtained results and observations, it is believed that

5
W.S. Barakat et al.
Al2O3 and compaction temperature influence the mechanical and
tribological properties of Al–Al2O3 coated Cu nanocomposites. In the
following section, the obtained results are discussed to highlight the
influence of coated Al2O3 content and compaction temperature on
properties of the produced nanocomposites. Also, the interplay between
microstructural, mechanical and tribological properties is discussed.
4. Discussion
4.1. Effect of Al2O3 coated Cu content
Generally, increasing reinforcement volume content improves
microstructural, mechanical and tribological properties if a homogenous
distribution of the reinforcement is achieved [3,13,16,29]. So, homog­
enous distribution of reinforcement phase in the matrix is a key
parameter for improving properties of the obtained nanocomposites.
Another important parameter that influence properties of nano­
composites is the voids in the sample which give indication on the
density of the produced samples. For samples compacted at 400 ᵒC,
increasing coated Al2O3 content, increases the micro-voids in the sample
(see Fig. 3) until formation of macro-voids in sample contain 15 wt%
coated Al2O3. In order to quantify the influence of coated Al2O3 addition
on the pores formation, the relative density versus Al2O3 content is
shown in Fig. 10. As shown in the figure, the relative density is decreased
to 94.1% for sample contain 10 wt% Al2O3 and consolidated at 400 ᵒC
while it reduces to 89.4% for sample contain 15 wt% Al2O3 which reflect
larger decreasing rate of relative density for this sample. This is due to
the agglomeration of coated Al2O3 nanoparticles during the consolida­
tion process (see Fig. 3(d)). The agglomeration of these particles in an
irregular shape results in more voids between Al and Al2O3 particles
[29]. For samples consolidated at 600 ᵒC, the relative density of sample
free of coated Al2O3 nanoparticles is almost 100% which mean that the
prepared sample is fully dense. Addition of 5 wt% coated Al2O3 de­
creases the relative density to 98.84% due to the higher compressive
Fig. 9. Coefficient of friction of Al–Al2O3 coated Cu nanocomposites consoli­
dated at two different temperatures: (a) 400 � C and (b) 600 � C.
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Composites Part B 175 (2019) 107140
properties of Al2O3 nanoparticles compared to Al which make the
consolidation of these composites harder than the pure metal. Addi­
tionally, the irregular shape of Al2O3 nanoparticles with sharp edges
results entrapping air between particles acting as pores. The relative
density decreasing rate is almost constant with increasing Al2O3 content
reaching 96.13% for sample contain 15 wt% Al2O3 nanoparticles which
indicates that the consolidation process is almost the same for all the
prepared composites (see Fig. 11).
The crystallite size is reducing with increasing Al2O3 content as
shown in Table 1. During high energy ball milling, two main mecha­
nisms occurs: initially, welding of Al particles entrapping between them
Al2O3 nanoparticles and fragmentation of the welded particles at longer
milling times [12,29]. So, during such experiment, two main reasons for
crystallite size reduction: the fragmentation of Al particles and the
entrapping of Al2O3 nanoparticles between Al particles which act as
impedance for dislocation movement. The presence of coated Al2O3
nanoparticles during high energy ball milling of Al particles results in
generation of dislocations and thus, the crystallite size is reduced [29,
30]. Additionally, during compaction at high temperature, the crystal­
lite size can be reduced as well due to the recrystallization of grains at
high temperature [31].
Microhardness of Al–Al2O3 coated Cu nanocomposites is observed to
be improved with increasing Al2O3 content up to 10 wt% for samples
compacted at 400 ᵒC despite the reduction in the relative density. It
increases from 47.5 HV for Al to 74.2 HV for Al-10 wt%Al2O3 coated Cu
nanocomposite achieving 56.2% increase. In these composites, two pa­
rameters affect the microhardness in an opposite manner. The reduction
of relative density negatively affects the general mechanical properties.
However, the grain refinement and dislocation generation strengthen
the composite. In these composites, the positive effect of grain refine­
ment and dislocation generation is able to vanish the negative effect of
relative density reduction. Therefore, this improvement in the micro­
hardness is attributed to the grain refinement/crystallite size reduction
(see Table 1). Additionally, the higher microhardness of Al2O3 nano­
particles and their coating layer (Cu nanoparticles) contribute this
improvement. Increasing Al2O3 content to 15 wt% results in a slight
reduction of the microhardness of the prepared composite due to the
agglomeration of Al2O3 nanoparticles (see Fig. 3(d)) and the larger
reduction of the relative density (see Fig. 10). So, in this sample, two
parameters negatively affect the mechanical properties against slight
grain refinement and crystallite size reduction (see Table .1). For the
samples compacted at 600 ᵒC, the microhardness is increased with Al2O3
content from 58.5 for Al to 120.4 for sample contain 15 wt% achieving
105% improvement. This large increase due to the higher grain refine­
ment and crystallite size reduction (see Table 1) besides the higher
hardness of Al2O3 and Cu particles as previously stated.
Fig. 10. Effect of Al2O3 content on relative density of Al–Al2O3 coated Cu
nanocomposites.
W.S. Barakat et al.
Fig. 11. Comparison between hardness improvement in the current samples
consolidated at 600 � C and available results in the literature.
In order to highlight the effect of Cu coating on the mechanical
properties, the microhardness of the samples consolidated at 600 � C was
compared with the properties of the same composite available in the
literature [9,13,22,32–34] without coating Al2O3. The figure represents
the improvement factor of microhardness by normalizing the micro­
hardness of the produced nanocomposites with the microhardness of the
raw Al. It is observed that the microhardness of Al–Al2O3 nano­
composites improves with increasing Al2O3 content up to a certain value
for all the compared samples. For Kang et al. [22] and Ezatpour et al.
[33] results, the maximum improvement is achieved at 5 wt% Al2O3,
while further increasing of the Al2O3 content results in microhardness
reduction. For the other materials shown in the figure (Wagih and Fathy
[9], Wagih [13], Mahbob et al. [32], Sadeghi et al. [34]), increasing
Al2O3 content more than 5%, the microhardness improvement rate is
reduced. Quantitively, the prepared composites in this study with 10
and 15 wt% Al2O3 coted Cu show the maximum microhardness among
the available results in the literature. Interestingly, the microhardness
improvement rate in the current study is constant up to 15 wt% Al2O3
which indicate that the microhardness can be improved by increasing
reinforcement weight fraction. This large and continuous improvement
in the current study is attributed to the coating of Al2O3 with Cu
nanoparticles which improve the surface properties, wettability and
dispersion of Al2O3 nanoparticles in Al matrix (see Figs. 1, 4 and 5).
The wear rate and coefficient of friction are highly influenced by the
addition of coated Al2O3 nanoparticles as shown in Figs. 8 and 9.
Generally, addition of Al2O3 nanoparticles reduces the wear rate for all
samples which indicates less material removal rate while the SiC parti­
cles penetrate the surface of the prepared nanocomposites. The presence
of Al2O3 coated Cu nanoparticles increases the impedance of the mate­
rial for SiC particles penetration which reduces the material removal
rate. Moreover, the improved hardness of Al–Al2O3 nanocomposites
than Al contributes the reduction of wear rate according to Archard law
[16,35–37]. For samples consolidated at 400 ᵒC, the major impact of
Al2O3 is observed at 5 wt%. A slight impact of Al2O3 content is observed
by increasing its content to 10 wt%. However, by increasing Al2O3
content to 15 wt%, the wear rate is increased again due to the agglom­
eration of Al2O3 nanoparticles in this composite (see Fig. 3 (d)). Addi­
tionally, the decrease of hardness of this material (see Fig. 7) contributes
the higher wear rate than sample contain 10 wt% Al2O3. This behavior
disappears in samples compacted at 600 ᵒC, at which, the wear rate is
reduced with increasing Al2O3 content. This result correlates well with
the hardness measurement (see Fig. 7) in which, the hardness is pro­
portional to Al2O3 content. The applied load during wear test influences
the wear rate as well. Increasing the applied load results in increased
wear rate because the penetration of SiC particle in the sample can be
simulated as indentation problem [3,29,38,39], at which increasing the
applied load results in larger indentation depth [39]. When the inden­
tation depth becomes larger than the critical indentation depth, large
debris are removed causing more plastic deformation of subsurface and
7
Composites Part B 175 (2019) 107140
facilitate the material removal process [40]. The coefficient of friction of
the prepared samples during abrasive wear test follow almost the same
trend observed for wear rates (see Fig. 9).
4.2. Effect of compaction temperature
Hot compaction process is presented in this work to consolidate the
milled powder instead of the conventional consolidation process, cold
compaction followed by sintering. Hot compaction process has advan­
tages over the conventional consolidation procedure such as shorter
processing time and less possibility for void formation. The compaction
temperature seems to highly influence physical, mechanical and wear
properties of Al–Al2O3 coated Cu nanocomposites. Increasing hot
compaction temperature provides more dense samples with less amount
of pores. It is observed in Fig. 10 that for the samples with the same
Al2O3 content, samples compacted at 600 ᵒC show larger relative density
than those compacted at 400 ᵒC. For example, the relative density of Al-
10 wt%Al2O3 coated Cu nanocomposite compacted at 600 ᵒC is 3.1%
larger than that compacted at 400 ᵒC. At higher compaction tempera­
ture, near Al melting temperature, plastic deformation of grains occurs
due to thermal stresses and consequently, the material flows easily to fill
the pores. Fig. 12 shows SEM micrograph of interface between four
grains and three grains in Al-10 wt%Al2O3 coated Cu nanocomposite
compacted at 400 and 600 ᵒC, respectively. As shown in the figure,
micro-pores are observed at the interface due to the low flowability of
the metal during hot compaction at 400 ᵒC. However, there is no evi­
dence on formation of micropores between grains in the sample com­
pacted at 600 ᵒC. Additionally, Al2O3 particles are found in small
agglomeration in sample compacted at 400 ᵒC (see Fig. 12(a)).
The crystallite size of the hot compacted samples is influenced by the
compaction temperature as shown in Table 1. For pure Al, samples
compacted at 600 ᵒC show larger crystallite size than those compacted at
400 ᵒC due to the recrystallization and grain growth occur during hot
compaction. Compaction of Al at 600 ᵒC, near the melting point, allows
the grain recrystallization and reduces the lattice strain due to grain
relaxation [31]. For samples contain Al2O3 nanoparticles, opposite trend
is observed, samples compacted at 600 ᵒC shows smaller crystallite size,
due to the presence of Al2O3 on the grain boundaries which creates
crystal defects such as dislocation buildup and prevents dislocation
movement and grain growth [13,41,42].
Microhardness of pure Al and Al–Al2O3 coated Cu nanocomposites is
dependent on the compaction temperature as shown in Fig. 7. For pure
Al, microhardness of samples compacted at 600 ᵒC is larger than for
samples compacted at 400 ᵒC, although, the crystallite size is larger. The
mechanical properties of compacted samples depend on the grain size of
the compacted material and the relative density [25,30]. The presence
of pores inside the material, reduces its resistance for penetration and
hence the hardness is reduced. So, for pure Al samples, the negative
effect of lower relative density on the hardness is dominant and over­
come the positive effect of smaller crystallite size. Unlike, samples
contain coated Al2O3 nanoparticles, the higher compaction temperature
Fig. 12. SEM micrograph of Al–10%Al2O3 coated Cu nanocomposite consoli­
dated at two (a) 400 � C and (b) 600 � C.
W.S. Barakat et al.
is, the larger microhardness is. For example, samples compacted at 600
ᵒ
C shows 24.9%, 38.2% and 71.7% larger hardness than samples contain
5, 10 and 15 wt% Al2O3 coated Cu nanoparticles compacted at 400 ᵒC,
respectively. This due to the smaller crystallite size of samples com­
pacted at 600 ᵒC (see Table 1) and the higher relative density (see
Fig. 10). Interestingly, for the sample with the largest Al2O3 content,
15 wt% and compacted at 600 ᵒC, microhardness is still improving
which is not the case of the sample compacted at 400 ᵒC due to the
prohibition of agglomeration (see Fig. 4) and the reduction of voids (see
Fig. 10). The prohibition of agglomeration and the better density of
samples compacted at 600 ᵒC results in better bonding between grains
which reduces the ability of the subsurface for plastic deformation
during indentation event [43,44].
The wear rate of Al–Al2O3 coated Cu nanocomposites compacted at
400 ᵒC and 600 ᵒC and measured at two different test load, 5 and 15 N is
replotted in Fig. 13 to highlight the effect of compaction temperature on
wear rates. Increasing hot compaction temperature, reduce the material
removal rate during wear test due to the better distribution of coated
Al2O3 nanoparticles and reduction of voids (see Fig. 12).
Based on the presented results and discussion, the hot compaction
temperature has large influence on the structural, physical, mechanical
and wear properties of Al–Al2O3 coated Cu nanocomposites. Increasing
compaction temperature results in better dispersion of Al2O3 nano­
particles in Al matrix which provide better impedance of dislocation
movement and hence less crystallite size. Additionally, this high tem­
perature allows higher flowability of the metal during hot compaction
process which reduces the probability to form voids and entrapping air.
The less void content provides better bonding between grains and
therefore less ability for plastic deformation which results in improved
hardness and wear properties.
5. Conclusion
Electroless deposition of Cu on Al2O3 nanoparticles followed by high-
energy ball milling and hot compaction was applied to manufacture
Al–Al2O3 coated Cu nanocomposites. Four different Al2O3 weight frac­
tions, 0, 5, 10 and 15 wt%, were considered to study the influence of
Al2O3 coated Cu nanoparticles addition on the properties of Al–Al2O3
nanocomposite. Additionally, hot compaction was applied at two
different temperatures, 400 ᵒC and 600 ᵒC to investigate the compaction
temperature effect on the properties of the sample. Structural, me­
chanical and wear properties of Al–Al2O3 coated Cu nanocomposite
were investigated.
Increasing Al2O3 coated Cu nanoparticles content in Al matrix
resulted in reduction of crystallite size due to the entrapping of these
particles between Al particles during ball milling which facilitate
Fig. 13. Effect of hot compaction temperature on wear rate of Al–Al2O3 coated
Cu nanocomposite. In the legend, 5 N and 15 N refer to the load during
wear test.
8
Composites Part B 175 (2019) 107140
fracture process and generate crystal defects. The relative density was
reduced by increasing Al2O3 content due to the formation of micropores
during consolidation process. Homogeneous dispersion of coated Al2O3
nanoparticles in Al matrix was achieved up to 10 wt% for sample
consolidated at 400 ᵒC, however increasing Al2O3 content to 15 wt%,
large particle agglomeration was occurred. For samples compacted at
600 ᵒC, good dispersion was achieved for relatively high Al2O3 content.
Microhardness increased with increasing Al2O3 achieving 105%
improvement for samples contain 15 wt% Al2O3 and compacted at 600
ᵒ
C due to the crystallite size reduction and well dispersion of Al2O3
nanoparticles. The improvement in hardness and crystallite size reduc­
tion improved the wear properties of Al–Al2O3 coated Cu
nanocomposites.
The properties of Al–Al2O3 coated Cu nanocomposites were highly
influenced by hot compaction temperature. The crystallite size of pure
Al was increased by increasing hot compaction temperature due to the
recrystallization and relaxation of grain caused by high temperature,
while, it decreased for Al–Al2O3 coated Cu nanocomposites. The
reduction of crystallite size was because of the presence of Al2O3
nanoparticles on the grain boundaries which prevent the grains relax­
ation and recrystallization. Increasing compaction temperature to 600 ᵒC
helped for achieving nanocomposite with higher Al2O3 content reaching
15 wt% without agglomeration which improves hardness by 105% and
reduce the wear rate by 52% compared to pure Al.
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