Materials Science & Engineering A 607 (2014) 188–196

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Fabrication of Al–2 vol% Al2O3/SiC hybrid composite via accumulative

roll bonding (ARB): An investigation of the microstructure and
mechanical properties
M. Reihanian a,n, F. Keshavarz Hadadian a, M.H. Paydar b
a
Department of Materials Science and Engineering, Faculty of Engineering, Shahid Chamran University of Ahvaz, Iran
b
Department of Materials Science and Engineering, School of Engineering, Shiraz University, Shiraz, Iran

art ic l e i nf o a b s t r a c t

Article history: An Al/Al2O3/SiC hybrid metal matrix composite was fabricated by accumulative roll bonding (ARB).
Received 22 January 2014 A mixture of Al2O3 and SiC (2 vol%) powders was poured between four Al layers during the first two ARB
Received in revised form cycles. The process was continued up to eight cycles without adding the powders in subsequent cycles.
24 March 2014
For comparison, non-reinforced (monolithic) Al was also processed by ARB under the same conditions.
Accepted 3 April 2014
At the initial stages, particle free zones as well as particle clusters were observed on the microstructure
Available online 13 April 2014
of the composite. After eight ARB cycles, a composite with a uniform distribution of particles was
Keywords: produced. At this stage, the tensile strength of the hybrid composite and the monolithic Al reaches to
Composites about 195 MPa and 150 MPa, respectively, about 5.3 and 4 times larger than that of annealed Al. The
Bulk deformation
hardness of the composite and the monolithic Al was measured as 83 and 58 VHN, respectively. Fracture
Bonding
surface after tensile testing revealed dimples at some regions after eight ARB cycles.
Mechanical characterization
& 2014 Elsevier B.V. All rights reserved.

1. Introduction dissimilar metals, named multilayer. During the co-deformation of

During the past two decades, researchers have been attracted
by metal matrix composites (MMCs) due to their excellent physical
and mechanical properties and their application in aerospace and
automotive industries [1,2]. Most MMCs are based on aluminum
because it is light and inexpensive in comparison with other
light metals, such as titanium and magnesium. Conventionally,
the manufacturing methods for MMCs can be classified into liquid-
state processing, semi-solid state processing and powder metal-
lurgy [1,2]. Some drawbacks of the conventional methods are
agglomeration, poor wet ability of the reinforcement, contamina-
tion and high manufacturing cost. In recent years, it has been
shown that accumulative roll bonding (ARB) is an effective tool for
manufacturing MMCs in the form of sheets. ARB is one kind of
severe plastic deformation that can produce sheet metals with
ultrafine-grained microstructure and superior properties [3]. ARB
consists of multiple cycles of stacking, rolling and cutting in which
large strains are imposed into the material without any change in
the cross section [4].
In general, MMCs can be fabricated by ARB with two different
routes. In the first route, the starting material consists of two or more
n
Corresponding author. Tel.: þ 98 611 3330010 19x5684; fax: þ98 611 3336642.
E-mail address: reihanian@scu.ac.ir (M. Reihanian).
dissimilar metals, necking occurs due to the differences in flow
properties of the constituent phases and further deformation causes
the hard phase to rupture. At a relatively large number of ARB cycle,
the hard phase is uniformly distributed within the matrix. Al/Mg [5],
Al/Ni [6], Al/Cu [7], Cu/Ag [8], Al/Zn [9], Cu/Zn [10] and Cu/Zn/Al [11]
are some examples of multilayer systems that have been produced
by this method. In the second route, ceramic powders such as B4C
[12,13], Al2O3 [14,15], SiC [16,17] and WC [18] are uniformly disper-
sed between the metal strips where they are stacked over each other.
ARB is then carried out to several cycles until a uniform distribution
of particles is achieved. It has been shown that, during ARB, a critical
reduction/strain is needed to get a uniform distribution of particles
within the matrix [19,20].
To date, many particulate MMCs that have been fabricated by
ARB contain a single reinforcement while only a slight attempt has
been made to fabricate hybrid composites whose microstructure
consists of two different types of reinforcements. To the authors'
knowledge, the hybrid MMCs that have been fabricated by this
method are Al/Al2O3/TiC [21], Al/Al2O3/SiC [22] and Al/Al2O3/B4C
[23–25]. Except for Ref. [23], the production of these hybrid
composites consists of a combination of ARB and anodizing
process. The procedure is to form a thin layer of Al2O3 on the Al
strip using anodizing process. Then, the anodized strip is placed
between the two surfaces of the Al strips, while the ceramic
particle is dispersed between the layers. During ARB, the anodized

http://dx.doi.org/10.1016/j.msea.2014.04.013
0921-5093/& 2014 Elsevier B.V. All rights reserved.
 M. Reihanian et al. / Materials Science & Engineering A 607 (2014) 188–196
layer is broken and finally a uniform distribution of the reinforce-
ments is achieved within the matrix.
In the present study, Al/Al2O3/SiC hybrid composite is fabricated
by ARB without using anodizing process as an additional process.
The Al2O3 and SiC powders are dispersed directly during the first
two cycles. The ARB process is carried out up to eight cycles. The
microstructure evolution and mechanical properties of the hybrid
composite are investigated by using the appropriate characteriza-
tion methods. The results are compared with annealed Al and with
monolithic Al processed by ARB at the same conditions.
2. Materials and methods
Particles of Al2O3 and SiC were used as reinforcements. The
powders were mixed through a milling process for 5 h under dry
conditions. The ball to powder weight ratio was 10 and the diameter
of the zirconia balls was 5 mm. Scanning electron microscope (SEM)
images of the particles before and after mixing are shown in Fig. 1.
Fig. 1. SEM images of the particles: (a) Al2O3, (b) SiC and (c) mixture of Al2O3 and SiC.
189
The average size of Al2O3 and SiC particles was about 1 mm and 5 mm,
respectively. As received commercially pure Al (AA1050) in the form of
a sheet with the thickness of 0.5 mm was used as the matrix material.
The chemical composition of the Al strip is presented in Table 1. The
strips were cut into 150 mm  70 mm and annealed at 400 1C for 2 h.
The annealed Al was considered as the base material at zero ARB
cycle. To set the prepared surfaces in contact and closely fixed to each
other, four holes were drilled near the edges of the strips. The
annealed strips were degreased by acetone and scratch brushed with
a circular stainless steel brush having a 0.3 mm wire diameter. To
fabricate the Al/Al2O3/SiC hybrid composite, ARB process was carried
out in two steps (Fig. 2). In the first step, 1 vol% mixture of Al2O3 and
SiC particles was uniformly distributed between the four layers of Al
strips (about 0.33 vol% between each layer). The stacked strips were
fastened at both ends by copper wires and rolled through a 50%
reduction in thickness at ambient temperature without lubrication.
The roll-bonded strip was then cut into two halves. Following the
preparation of the surfaces, two strips were stacked and roll-bonded
again under the same conditions as the first cycle, while 1 vol%
190 M. Reihanian et al. / Materials Science & Engineering A 607 (2014) 188–196

Table 1
Chemical composition (wt%) of the materials used in this study.

Al (balanced)

Be Ti Ni Cr Zn Mg Mn Cu Fe Si

0.0001 0.0141 0.005 0.0024 0.005 0.0002 0.0061 0.0036 0.252 0.0752

Pb Li Ca B Zr Bi Na V Sr Sn

0.002 0.0001 0.0005 0.0005 0.002 0.005 0.0015 0.0131 0.0001 0.001

In Hg Ag Co Cd Ga

0.01 0.003 0.001 0.003 0.001 0.0094

Fig. 2. Schematic illustration of ARB process used to fabricate hybrid composite.

mixture of Al2O3 and SiC particles dispersed between them. After this
step, the total amount of the Al2O3 and SiC reached to 2 vol% and the
thickness of the composite sheet was about 1 mm. In the second step,
ARB was repeated up to six cycles (eight cycles in total) without
adding the particles between the layers. ARB was conducted with a
rolling machine having the capacity of 20 t and rolling diameter of
170 mm. The rolling speed was set to 12 rpm.
For tensile testing, samples with orientation along the rolling
direction were machined from the ARB processed strips. The gauge
width and length of the samples were 2.8 and 8 mm, respectively.
Tensile test was done at room temperature with a tensile testing
machine under a nominal initial strain rate of 4  10  4 s  1. The
percent elongation was obtained by measuring the difference
between the gauge length before and after the tensile test. Vickers
hardness method was used for hardness testing. The hardness
measurements were taken by applying a load of 30 kgf for 10 s on
the surface of the strip surfaces. Field emission scanning electron
microscope (FESEM) equipped with energy dispersive spectroscopy
(EDS) was used to investigate the microstructure on the normal
direction–rolling direction (ND–RD) sections and fracture surfaces.
3. Results and discussions
3.1. Microstructure evolution
Fig. 3 illustrates a typical SEM image of the Al/Al2O3/SiC hybrid
composite and the corresponding EDS analysis used to identify the
 M. Reihanian et al. / Materials Science & Engineering A 607 (2014) 188–196
type of particles in the Al matrix. The EDS results corresponding to
the exhibited points are indicated by arrows. Results indicate that
the small and white particles are alumina while large and gray
particles are silicon carbide.
SEM micrographs of the Al/Al2O3/SiC hybrid composite after
various ARB cycles are shown in Fig. 4. It is observed that at the
initial stages of ARB (Fig. 4a and b), the distribution of particles is
non-uniform and the microstructure consists of large clusters as
well as particle free zones. As the ARB proceeds (Fig. 4c), clusters
and particle free zones disappear to some extent and finally after
eight cycles (Fig. 4d), a uniform distribution of Al2O3 and SiC
particles is observed in the Al matrix.
The mechanisms responsible for particle distribution through
ARB are regarded as follows. During ARB, the number of layers
increases while their thickness decreases [4]. When four 0.5 mm
thick strips are roll bonded up to eight cycles with a 50% reduction
per cycle, the number of layers increases to 1024 and their
thickness reduces to 1.9 mm. At the same time, Al matrix deforms
plastically and extrudes through the particles owing to separation
and movement of the particles from interfaces into the bulk of the
aluminum matrix. In addition, it has been reported that elongation
of the clusters in the rolling direction can increase the distance
between the particles inside the clusters [26], changing the dense
clusters into the diffuse clusters [23]. Dense clusters are defined as
agglomerations in which no matrix material is present between
the particles. Clusters with some amount of the matrix material
between the particles are referred to as diffuse clusters. Another
mechanism that is considered for dispersion of the particles is that
[27], at the initial stages, the particle layers are split to small pieces
or fragments. During deformation, fragments of particles behave
Fig. 3. (a) Typical SEM image of hybrid composite after four ARB cycles used to identify the particles, (b) and (c) EDS results corresponding to points A and B, respectively.
191
as a hard phase and the soft matrix flows through them. As a
result, the particles adjacent to the fragment–matrix interfaces
move along the interface of the fragments. The number of the
particles being removed from the fragment surfaces increases with
increasing the ARB cycle. Accordingly, clusters become progres-
sively thinner and orient along the rolling direction, leading to
dispersion of the particles in the matrix.
The critical reduction to get a uniform distribution of particles
in MMCs produced by ARB has been modeled previously [19,20].
According to the model, for a hybrid composite containing two
different particles of A and B, the critical reduction can be
determined through an equation of the form [20]
" #1=3  
π dA dB
Rcr ¼ 1  ð1Þ
3 3
6ðf A d þf B d Þ to
B A
where d is the particle size, f is the volume fraction and t o is the
initial thickness of the layers. The subscripts A and B stand for
particles A and B, respectively.
For dA ¼1 mm, dB ¼5 mm, f A ¼ f B ¼ 0:01 and t o ¼ 0:5 mm, the
model predicts that to obtain a uniform distribution of particles in
a hybrid composite, a total reduction of at least 0.9925 is required.
After eight ARB cycles, a 0.996 total reduction is applied, which is
larger than the predicted critical strain. Therefore, a uniform
distribution of Al2O3 and SiC is expected after these cycles.
Fig. 5 illustrates the low magnification SEM images of the
composite microstructure at different ARB cycles. The dark area in
every image of Fig. 5 is the mounting material. The difference in the
sheet thickness is due to spread of the mounting material on the
surface of the strips. Therefore, the sheet thickness of the strips
192 M. Reihanian et al. / Materials Science & Engineering A 607 (2014) 188–196
Fig. 4. SEM micrographs of the hybrid composite after various ARB cycles; (a) two, (b) four, (c) six and (d) eight cycles.
appears to be different. Inspection of Fig. 5 reveals that at the initial
cycles (Fig. 5a and b), the microstructure contains several porosities.
These porosities may be created between the layer interfaces or
between the Al matrix and ceramic particles [28]. The shape of the
porosities is rather irregular after two cycles (Fig. 5a) and becomes
elongated in the rolling direction after four cycles, (Fig. 5b). The
amount of porosity reduces to some extent after six cycles (Fig. 5c).
As the ARB continues to eight cycles, the porosities are removed
from the microstructure and the bonding at interfaces improves
sufficiently. Among the many mechanisms, it has been reported
that the film theory is the major mechanism of bonding at low
temperature deformations [29]. According to this mechanism, the
fracture of the work-hardened surface layer or oxide film and the
extrusion of virgin metal through the cracks have the major role in
the real contact between metals. Bonding can be obtained when the
deformation causes fresh metal surfaces to be exposed. Ceramic
particles may act as barriers to film theory and inhibit the creation
of good bonding [13]. On the other hand, plastic deformation of the
matrix through particles can facilitate fresh metal surfaces to be
exposed. At the same time, rolling pressure supplies sufficient force
and can create large contact areas. Therefore, good bonding can be
achieved at high ARB cycles even in the presence of ceramic
particles.
3.2. Mechanical properties
The engineering stress–strain curves of Al/Al2O3/SiC hybrid
composite at various ARB cycles are shown in Fig. 6. For compar-
ison, the engineering stress–strain curve of the annealed Al and
monolithic (pure) Al are also included. The variations of ultimate
tensile stress (UTS) and percent elongation (% el.) with the number
of ARB cycles are plotted in Fig. 7. The properties at zero cycle
correspond to the annealed Al. It is observed that the UTS of the
monolithic Al and the hybrid composite increases noticeably with
increasing the number of ARB cycle. The UTS of the hybrid
composite is larger than that of the pure Al at all cycles. After
eight cycles, the UTS of the hybrid composite and the monolithic
Al reaches to 195 MPa and 150 MPa, respectively, about 5.3 and
4 times larger than that of annealed Al.
 M. Reihanian et al. / Materials Science & Engineering A 607 (2014) 188–196
Fig. 5. Low magnification SEM images of the hybrid composite after various ARB cycles; (a) two, (b) four, (c) six and (d) eight cycles.
Fig. 6. The engineering stress–strain curves of the annealed Al, monolithic Al and
hybrid composite.
193
It has been reported that strain hardening and grain refinement
are two major strengthening mechanisms that increase the
strength of a metal during SPD process [30,31]. Strain hardening
results from the increase in dislocation density within the grains
or is due to the formation of low angle dislocation boundaries [30].
This is the dominant mechanism at the initial stages of SPD
methods [3]. At the final stages, the misorientation of the disloca-
tion boundaries reaches to high angles and grain refinement to the
ultra-fine scale causes the increase in the strength [31]. In addition
to these mechanisms, other strengthening mechanisms can
also contribute to the strengthening of the composite due to the
presence of ceramic particles.
One important mechanism that explains the strengthening due
to dispersion of particles involves dislocations bowing (Orowan
looping) around the particles [32]. Dispersion of fine particles are
an effective mechanism of strengthening in which the dislocations
extrude between the particles, leaving dislocation loops around
them. These loops effectively decrease the mean particle spacing
194 M. Reihanian et al. / Materials Science & Engineering A 607 (2014) 188–196
Fig. 7. Variation of UTS and percent elongation of the monolithic Al and hybrid
composite with the number of ARB cycles; the properties at zero cycles correspond
to annealed Al.
and increase the stress required for movement of subsequent
dislocations. This explains the higher rate of strain hardening
in the particle-reinforced composite compared with a monolithic
material.
Other contributions of particles to strengthening mechanism
arise from the difference in flow properties of the matrix and
particles. Since the particles are non-deformable and the matrix
deforms plastically, a strain incompatibility is generated between
the particles and the matrix [33]. The strain incompatibility leads
to the generation of geometrically necessary dislocations that are
stored in the matrix, near the particle–matrix interfaces. Geome-
trically necessary dislocations are in addition to those stored
statistically in the matrix and can accommodate the strain gra-
dients and incompatibility between the particle and the matrix.
The presence of particles may also produce extra (secondary)
dislocations during deformation [34,35]. These dislocations are
generated due to activation of the further slip systems near the
particle–matrix interfaces to accommodate the deformation and
impede the motion of primary glide dislocations.
The variation of percent elongation with the number of ARB
cycles shows that the percent elongation of the composite and
monolithic Al decreases remarkably after the first ARB cycle. The
percent elongation at zero cycle (annealed Al) is about 35%. After the
initial cycles, it is reduced to less than 5% for the monolithic Al and
for the hybrid composite. The sharp decrease in percent elongation
results from the large increase in dislocation density and the
accumulation of internal stresses that promote the nucleation of
cracks. This trend can be observed by percent elongation at the initial
stages of each SPD process [36]. The percent elongation rises slightly
with increasing the number of ARB cycle. This can be attributed to
the increase in bonding during ARB. The bonding at interfaces can
increase the elongation by delaying crack formation at the layer
interface as well as the particle–matrix interface. The elongation is
also increased when the distribution of particles in the hybrid
composite becomes uniform because the net distance between the
particles is increased and the probability of joining cracks at particle
sites is reduced. It is noted that the percent elongation of the hybrid
composite is lower than that of monolithic Al because particles act as
effective sites for crack nucleation [33].
The variation in hardness with the number of ARB cycle is
presented in Fig. 8. For comparison, the hardness of annealed Al is
also included. A similar trend like UTS is observed for hardness,
that is, the hardness increases with increasing the number of ARB
cycle. The mechanisms that are attributed to the hardness varia-
tions are similar to those discussed for UTS. For annealed Al, the
Fig. 8. Hardness variation of the monolithic Al and hybrid composite with ARB
cycle; the hardness at zero cycles corresponds to annealed Al.
average hardness is 20 VHN. After eight ARB cycles, the average
hardness reaches to 58 VHN and 83 VHN for monolithic Al and
hybrid composite, respectively. However, the hardness of the
hybrid composite rises with a higher rate which is due to the
higher rate of strain hardening in hybrid composite compared
with the monolithic Al. Similar trend in hardness variation has also
been reported for other MMCs fabricated by ARB [14,16,27].
It is noted that, the hardness values for pure Al only slightly
increase from four to eight ARB cycles while the UTS increases
significantly. It has been demonstrated that the hardness of the
ARB processed materials is affected by several factors such as
oxide layer at interfaces, depth of the removed material during
surface preparation and load/indentation depth. Therefore, the
measured hardness of the sheet can overestimate or underesti-
mate the averaged hardness of multiple layers [37]. On the other
hand, tensile strength is a bulk property and is not influenced by
these factors at all. As a result, it is expected that the increase in
hardness is not necessarily the same as the increase in the UTS.
3.3. Tensile fracture surface
The tensile fracture surface of the annealed Al together with
monolithic Al and hybrid composite are illustrated in Fig. 9. The
fracture surface of the annealed (Fig. 9a) and monolithic Al (Fig. 9b)
reveals several equiaxed and small dimples. Due to unequal triaxial
stresses, some dimples are elongated in one or other directions.
These appearances are the characteristics of a typical ductile fracture.
Each dimple corresponds to a crack nucleation site, which has been
linked up by plastic deformation process.
Comparison of Fig. 9a and b indicates that the dimples in
monolithic Al distribute more closely, meaning that a lower amount
of Al matrix exists between them. This can be due to the extensive
work hardening and lower ability of the monolithic Al for plastic
deformation. In hybrid composite, void nucleation and growth starts
at particle–matrix interface as well as in the matrix (Fig. 9c). The
dimples that are nucleated at the particle sites (indicated by circle)
are considerably deeper and larger than that initiated at other
locations. The particles responsible for the void nucleation can be
observed at the bottom of these dimples, indicating that particles are
suitable sites for crack initiation and propagation. The size, separa-
tion, and interfacial bonding of these particles determine the overall
propagation characteristics of ductile cracks and, therefore, the
ductility of the material. The low percent elongation of hybrid
composite can be a result of extensive void nucleation and the
greater ease with which void link up is affected when the particles
 M. Reihanian et al. / Materials Science & Engineering A 607 (2014) 188–196
Fig. 9. Tensile fracture surface of (a) annealed Al, (b) monolithic Al and (c) hybrid composite after eight ARB cycles.
are present. The ductile fracture appearance is also reported for other
MMCs fabricated by ARB [14,21,22,27].
4. Conclusions
 Al/Al2O3/SiC hybrid composite is successfully produced in the
form of sheet through ARB process. A uniform distribution of
particles is not observed in the microstructure except for
sufficient high ARB cycles (eight cycles).
 Several irregular porosities are observed at low ARB cycles and
become elongated at intermediate cycles. After eight cycles, the
porosities are considerably removed from the microstructure.
From the SEM investigations, the conclusion is drawn that the
bonding at interfaces improves sufficiently during the last
stages, which can be discussed by means of the thin film
theory.
 The tensile strength of the hybrid composite rises with increas-
ing the number of ARB cycles and is larger than that of
monolithic Al. It can be concluded that additional strengthen-
ing mechanisms have contributed to the presence of the
195
particles in the hybrid composite. A similar trend is observed
for hardness variation. After eight cycles, the strength and
hardness of the hybrid composite reaches 95 MPa and 83
VHN, respectively.
 After the initial ARB cycles, the percent elongation decreases
remarkably due to considerable strain hardening. As the ARB
proceeds, the percent elongation increases slightly, which can
be contributed to the removal of the porosities and the increase
in bonding.
 SEM observation of the fracture surface reveals large and deep
dimples at the fracture surface of the hybrid composite,
indicating that particles have a significant effect on the ductility
of the hybrid composite.
Acknowledgment
The authors would like to acknowledge the financial support of
Shahid Chamran University of Ahvaz through the Grant number
EN-92-874095.
196 M. Reihanian et al. / Materials Science & Engineering A 607 (2014) 188–196
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