Microstructure and mechanical properties of

Al/Al2O3 MMC produced by anodising and

cold roll bonding
R. Jamaati* and M. R. Toroghinejad
In the present paper, Al–Al2O3 composite strips are produced by the cold roll bonding process of
anodised aluminium strips. This technique has the flexibility to control the volume fraction of metal
matrix composites by varying the oxide layer thickness on the anodised aluminium strip.
Microhardness, tensile strength and elongation of composite strips are investigated as a function
of quantity of alumina and the applied production method. It is found that higher quantities of
alumina improve microhardness and tensile strength, while the elongation value decreases
negligibly. Furthermore, prerolling annealing is found to be the best method of producing this
composite via the cold roll bonding process. Finally, it is found that both monolithic aluminium and
aluminium/alumina composite exhibited a ductile fracture, having dimples and shear zones.
Keywords: Metal matrix composite, Cold roll bonding, Anodising, Microstructure, Mechanical properties

Introduction To date, this method has been widely used for

There has been a wide interest in developing metal
matrix composites (MMCs) due to their unique mechan-
ical properties, such as light weight and high elastic
modulus. The common fabrication routes of particulate
reinforced MMCs include spray deposition, liquid
metallurgy and powder metallurgy.1,2 Since expensive
equipment is required and the processing routes are
usually complex, the high cost of producing MMCs
using these methods has limited the application of MMC
materials.
Among the current composite material technologies,
cold roll bonding (CRB) for producing composite sheets
and foils has experienced rapid growth and development
in recent years owing to its efficiency and economic
considerations. Cold roll bonding is a solid phase
welding process, in which bonding is established by
joint plastic deformation of the metals to be bonded.
Bonding is obtained when the surface expansion breaks
the oxide layers, and the roll pressure bonds the surfaces
together causing the material to be extruded through
cracks in the fractured oxides, if present.3–7
CRB is also referred to by different authors as ‘cold
pressure welding by rolling’,8 ‘bonding by cold rolling’,9
‘clad sheet by rolling’,10 and cold roll bonding.3–7 This
process can be used with a large number of materials. In
addition, materials that cannot be bonded by traditional
fusion often respond well to CRB. Compared with other
methods, CRB is of low cost and simple, and can be
easily automated.
Department of Materials Engineering, Isfahan University of Technology,
Isfahan 84156–83111, Iran
26 August 2010
*Corresponding author, email r.jamaatikenari@ma.iut.ac.ir
producing dissimilar layered composites, including Al–
steel,11 Al–Zn,12 Al–Ti (Ref. 13) and Al–Ni.14 In addi-
tion, the authors have produced MMCs by continual
annealing and roll bonding15,16 and accumulative roll
bonding17,18 processes. These MMCs exhibited excellent
microstructure and mechanical properties, but the
production methods were costly. However, there is no
conclusive research either on the production of MMCs
with different quantities of reinforcement by anodising
and CRB processes or on the effects of different annealing
treatments (pre- and post-rolling) on the MMC micro-
structure and mechanical properties.
The aim of the present study was to manufacture the
Al–Al2O3 composite via anodising and CRB processes
and to investigate the composite’s microstructure
and mechanical properties, such as tensile strength and
microhardness. In addition, the effects of pre- and post-
rolling annealing treatments on microstructure and
mechanical properties were examined.
Experimental
As received commercial purity aluminium sheets were
cut into 20065060?4 mm strips parallel to the sheet
rolling direction. Furthermore, some of the specimens
were annealed at 643 K for 2 h (specifications are given
in Table 1).
Some of the as received and annealed strips were
anodised in 15 wt-% sulphuric acid under an applied
voltage of 16 V for two different times (5 and 60 min) to
generate two extra oxide film thicknesses. Before
anodising, the specimens were cleaned in NaOH and
then in a HNO3 bath. Chemical compositions of the
baths are given in Table 2. To ensure a constant and
homogeneous temperature throughout the solution,

ß 2011 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 26 August 2010; accepted 18 October 2010
1648 DOI 10.1179/1743284710Y.0000000011 Materials Science and Technology 2011 VOL 27 NO 11
 Jamaati and Toroghinejad
1 Schematic illustration of principle of CRB for producing
composite
forced convection was provided by electrolyte stirring.
These oxide layers were formed at a low electrolyte
temperature (16uC) favouring rapid growth and reduced
dissolution of the oxide layer. Then, strips were
neutralised in ammonium acetate (Table 2) under an
applied voltage of 16 V for 15 min, to enhance bonding
in the CRB process. The thickness of the alumina layers
obtained by the anodising process was determined by
scanning electron microscopy (SEM) of the oxide cross-
sections. Average and standard deviations of y20
measurements were calculated.
The schematic illustration of the CRB process is
shown in Fig. 1. First, the two annealed strips (non-
anodised) were surface prepared. A number of authors
have claimed degreasing followed by scratch brushing
with a rotating steel brush to be the best method for
surface preparation.6,19 Therefore, the preparation
processes for some of the (non-anodised) strips in the
present study included degreasing in an acetone bath
followed by scratch brushing using a stainless steel brush
with wires 0?26 mm in diameter. The initial surface
roughness of the specimens was 0?5 mm, which, after
scratch brushing, rose up to y4?2 mm in the long-
itudinal and transverse rolling directions. Then, the
anodised strip was laid between the prepared surfaces of
strips. The strips were stacked over each other, fastened
at both ends and roll bonded with a specific reduction
percentage equal to 60%. The final thickness of the as
rolled samples was y0?4 mm. Generally, the time
between surface preparation and rolling was kept to
,120 s. Care was taken to properly align the two strip
surfaces before rolling. The CRB experiments were
carried out with no lubrication, using a laboratory
Table 1 Specifications of commercial purity Al
Chemical Tensile
composition, strength,
Material wt-% Condition MPa
Al 1100 99.11Al, 0.17Si, As received 157.4
0.49Fe, 0.12Cu, Annealed 84.5
0.02Mn, 0.09
others
Microstructure and mechanical properties of Al/Al 2 O 3 MMC
rolling mill, with a loading capacity of 20 tons. The roll
diameter was 125 mm, and the rolling speed was set at
2 m min21. A number of the samples were annealed at
643 K for 2 h before or after the CRB process to
investigate the effects of pre- and post-rolling annealing
on mechanical properties.
The microstructures of the CRB processed composite
strips under various conditions were evaluated by
optical microscopy (OM) and SEM Philips XL30. To
evaluate alumina distribution in the matrix and the
bonding conditions of the CRB processed composite
strips, optical examination of the strips was conducted.
All optical microstructures were observed along the
rolling direction–normal direction (RD–ND) plane of
the strips. To evaluate the alumina layer thickness after
anodising and before CRB process and investigation of
the fracture surfaces after tensile test, SEM examination
of strips was conducted.
Vickers microhardness of the samples was measured
under a load of 100 g. Microhardness was measured
randomly at 10 different points on the strips for each
sample, the maximum and minimum results were
disregarded and the mean microhardness value was
calculated using the remaining eight values.
The tensile test specimens were machined from the
rolled strips according to the ASTM E8M tensile
sample, oriented along the rolling. The gauge width
and length of the tensile test specimens were 6 and
25 mm respectively. The tensile tests were conducted at
ambient temperature on a Hounsfield H50KS testing
machine at an initial strain rate of 1?6761024 s21.
Three tensile tests were performed with each sample.
Total elongation of the sample was measured as the
difference in gauge length before and after testing.
Results and discussion
Microstructure observation
Figure 2 demonstrates the SEM image of the RD–ND
plane of the strips anodised for 60 min before subjecting
to the CRB process. It is clear that the alumina layer has
formed on aluminium strip. The thickness of this layer
throughout the strip is constant, which is one of the
advantages of the anodising process. As mentioned
before, the alumina layer thicknesses on aluminium strips
anodised for 5 and 60 min were about 5?1¡0?2 mm and
16¡0?5 mm, which are equal to 1?13 and 3?55 vol.-%
respectively.
Figure 3 illustrates the OM images of the microstruc-
tures of the 3?55 vol.-% composite strips produced by
the CRB process for production methods. For as
received and post-rolling annealed samples, the alumina
particles are larger and non-uniformly distributed in the
matrix compared to the prerolling annealed sample.
During rolling process, the aluminium matrix plastically
Yield
strength, Elongation, Microhardness,
MPa % HV0.1
142.3 7.2 48
39.3 37.8 19
Materials Science and Technology 2011 VOL 27 NO 11 1649
Jamaati and Toroghinejad Microstructure and mechanical properties of Al/Al 2 O 3 MMC

2 Image (SEM) of RD–ND plane of 60 min anodised strip

deforms and extends, the but alumina layer is very

brittle and can respond to stress by necking, fracturing
and separation phenomena. Therefore, the alumina
layer breaks up into particles or platelets, and it is
consequently uniformly distributed in the aluminium
matrix. Owing to the cracks that open up in the alumina
layer, aluminium flows through the fractured alumina
regions. The interface, therefore, is a combination of
oxide fragments and bonded areas of extruded alumi-
nium. Consequently, the cracking of the alumina layer
allows metal–metal contact and roll bonding to take
place. The matrix of the prerolling annealed sample can
open all the cracks in the alumina layer due to high
plasticity, which subsequently allows stronger bonding
to take place when compared with the as received and
post-rolling annealed samples. It is important and
interesting to note that in as received composite strip,
dominant phenomenon is necking, while for post-rolling
annealed sample, both necking and fracturing are
dominant phenomena. Finally, in prerolled annealed
composite strip, all three phenomena (necking, fractur-
ing and separation) take place, and therefore, an MMC
with a uniform particle distribution and fine particle size
is produced. Based on the above results, it can be
concluded that prerolling annealing is a good alternative
method for producing the Al–Al2O3 composite by the
CRB process.
Figure 4 shows the OM images of the microstructures 3 Images (OM) of composite strips with 3?55 vol.-% pro-
of the composite strips produced by the CRB process duced by CRB process for a as received, b post-rolling
with two alumina quantities for the prerolling annealing annealed and c prerolling annealed samples
method. It can be seen that by increasing the amount of
alumina, particle size increases but uniformity decreases. minimum values of microhardness were obtained for the as
In other words, by decreasing the thickness of the received (95, 104 and 119 HV) and post-rolling annealed
alumina layer in the anodising process, this layer breaks (34, 39 and 43 HV) strips as seen in Fig. 5. In other words,
up more easily during the rolling, which leads to the greatest value of microhardness was achieved when the
improved uniformity. strip was rolled without pre- or post-rolling annealing
treatment. For post-rolling annealed strips, a remarkable
Mechanical properties decrease was achieved in microhardness, which was almost
Figure 5 shows variations in microhardness versus quan- three times that of the strip before post-rolling annealing
tity of alumina for different production methods. It should treatment. This may be related to the significantly
be noted that microhardness measurements were per- decreased amount of dislocations and dislocation debris
formed on one-third thickness of samples. Maximum and after annealing treatment and the consequent decrease in
workhardening. From Fig. 5, it is obvious that the
Table 2 Specifications of baths used microhardness value improved when the alumina quantity
Bath Chemical composition increased. For as received and prerolling annealed samples,
this is attributed to reinforcing role of alumina particles in
NaOH 60 g L21 NaOHz120 g L21 Al3zz the aluminium matrix, which results in additional strain
10 g L21 additives hardening in the matrix and, therefore, increasing the
HNO3 50 wt-% HNO3zH2O microhardness. For the post-rolling annealed sample,
Ammonium acetate 2 g L21 NH4CH3COOzH2O
improving the microhardness with increasing the alumina

1650 Materials Science and Technology 2011 VOL 27 NO 11

 Jamaati and Toroghinejad
4 Images (OM) of composite strips produced by CRB process for prerolling annealing method with a 1?13 vol.-% and
b 3?55 vol.-% alumina
quantity is related to strain hardening as a result of the
mismatch between the matrix and the particles in terms of
their coefficients of thermal expansion. Thermal expansion
coefficients for aluminium and alumina are 22?261026
and 5?461026 m mK21 respectively. Furthermore, the
value of microhardness error bars increased by increasing
alumina particles. In other words, the values of micro-
hardness obtained for cold roll bonded strips without
alumina particles are very close. This can be related to the
non-uniform distribution of particles with higher quan-
tities of Al2O3 particles.
Figure 6 presents the stress–strain curves for the Al–
Al2O3 composites produced by the CRB process with
various quantities of alumina using the prerolling
annealing method, a monolithic aluminium (without
alumina particles) produced by the same process and an
annealed aluminium used as the raw material. According
to Fig. 6, tensile strength values for the Al–3?55 vol.-
%Al2O3 composite and monolithic and annealed samples
were equal to 256, 201 and 84 MPa respectively. In fact,
the composites have a higher tensile strength than the
monolithic and the annealed aluminium strips so that the
tensile strength of the composite (with 3?55 vol.-%
alumina particles) is 1?3 and 3?1 times higher than that
obtained for the monolithic and annealed aluminium
5 Variations in microhardness versus alumina quantity
with different methods
Microstructure and mechanical properties of Al/Al 2 O 3 MMC
strips respectively. This is while the elongation value
decreases negligibly. Furthermore, it can be seen that
tensile strength increases by increasing the quantity of
alumina in the matrix. These results are related to the
following two main effects of alumina particles:
(i) during the tensile test, alumina particles act as a
barrier to dislocation movement, causing
enhancement of strength15–18,20
(ii) presence of alumina particles in the soft alumi-
nium matrix generates dislocation to pile up in
their neighbourhood.
Therefore, dislocation density in the matrix near the
aluminium/alumina interfaces increases to enhance
strength. In other words, pinning the dislocations and
impeding their motion by alumina particles results in
enhanced dislocation density, in dislocation–dislocation
interactions and, thereby, in improved strength.15–18,20
Fracture surfaces of monolithic aluminium and Al–
3?55 vol.-%Al2O3 composite produced by prerolling
annealing after tensile test are presented in Fig. 7.
Regarding Fig. 6, the tensile elongation of the composite
strip is lower than that of the monolithic aluminium.
This is attributed to presence of Al/Al2O3 interfaces,
which act as crack source and crack propagation during
tensile test (Fig. 7b). In fact, it has been reported1 that
the failure of composite materials is related to void
6 Stress–strain curves of annealed and monolithic alumi-
nium as well as Al–Al2O3 composites produced by pre-
rolling annealing with 1?13 and 3?55 vol.-% alumina
Materials Science and Technology 2011 VOL 27 NO 11 1651
Jamaati and Toroghinejad Microstructure and mechanical properties of Al/Al 2 O 3 MMC
7 Fracture surfaces after tensile test for a monolithic aluminium and b composite with 3?55 vol.-% alumina
formation in the matrix within reinforcement/matrix
interface, and therefore, the elongation of composites
decreased compared to pure materials. In addition,
higher volume fraction of alumina causes more void
formation and strain hardening during plastic deforma-
tion, and as a result, the ductility decreases.
Figure 7 also reveals that both monolithic aluminium
and Al–Al2O3 composite exhibited a ductile fracture,
having dimples and shear zones. This kind of fracture
occurs by formation and coalescence of microvoids ahead
of the crack and very limited dislocation activity.16,17 It is
important that for monolithic sample, the quantity and
depth of dimples is higher compared to that for composite
sample. This is attributed to additional strain hardening
due to the presence of alumina particles in aluminium
matrix for composite sample.
Conclusions
The present work investigated the effects of quantity of
alumina particles produced by anodising and the
production method of Al–Al2O3 composite using the
CRB process on the microstructure and mechanical
properties of the product. The findings can be sum-
marised as follows.
1. For the as received and post-rolling annealed
samples, the alumina particles were larger and non-
uniformly distributed in the matrix compared to the
prerolling annealed specimen. Furthermore, by decreas-
ing the thickness of the alumina layer in the anodising
process, this layer breaks up more easily during the
rolling to enhance uniformity.
2. Microhardness increased with increasing alumina.
Furthermore, the highest values for microhardness were
obtained in the as received strips (without pre- and post-
rolling annealing treatments).
3. The tensile strength of the cold roll bonded strips
increased with increasing alumina. Furthermore, elonga-
tion improved negligibly with decreasing alumina
content.
1652 Materials Science and Technology 2011 VOL 27 NO
4. Prerolling annealing was identified as the best
method for producing Al–Al2O3 composite strips via the
CRB process.
5. Both monolithic aluminium and Al–Al2O3 compo-
site exhibited a ductile fracture, having dimples and
shear zones.
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