Materials and Design 51 (2013) 367–374

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Materials and Design

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

Accumulative press bonding; a novel manufacturing process

of nanostructured metal matrix composites
Sajjad Amirkhanlou a, Mostafa Ketabchi a,⇑, Nader Parvin a, Shohreh Khorsand b, Reza Bahrami a
a
Department of Mining and Metallurgical Engineering, Amirkabir University of Technology, Tehran, Iran
b
Young Researchers and Elite Club, Najafabad Branch, Islamic Azad University, Najafabad, Isfahan, Iran

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

Article history: A new manufacturing process for metal matrix composites has been invented, namely accumulative press
Received 22 February 2013 bonding (APB). The APB process provided an effective method to produce bulk Al/10 vol.% WCp composite
Accepted 9 April 2013 using tungsten carbide (WC) powder and AA1050 aluminum sheets as the raw materials. The microstruc-
Available online 18 April 2013
tural evolutions and mechanical properties of the monolithic aluminum and Al/WCp composite during
various APB cycles were examined by scanning electron microscopy, X-ray diffractometry, X’pert High-
Keywords: Score software, and tensile test equipment. The results revealed that by increasing the number of APB
Accumulative press bonding
cycles (a) the uniformity of WC particles in aluminum matrix improved, (b) the porosity of the composite
Metal matrix composites
Nanostructured materials
eliminated, (c) the particle free zones decreased and (d) the cluster characteristics improved. Hence, the
Mechanical properties final Al/WCp composite processed by 14 APB cycles showed a uniform distribution of WCp throughout the
aluminum matrix, strong bonding between particles and matrix, and a microstructure without any poros-
ity and undesirable phases. The X-ray diffraction results also showed that nanostructured Al/WCp com-
posite with the average crystallite size of 58.4 nm was successfully achieved by employing 14 cycles of
APB technique. The tensile strength of the composites enhanced by increasing the number of APB cycles,
and reached to a maximum value of 216 MPa at the end of 14th cycle, which is 2.45 and 1.2 times higher
than obtained values for annealed (raw material, 88 MPa) and 14 cycles APBed monolithic aluminum
(180 MPa), respectively. Though the elongation of Al/WCp composite lessened during the initial cycles
of APB process, it increased at the final cycles of the mentioned process by 78%. Role of WC particles, uni-
formity of reinforcement, porosity, bonding quality of the reinforcement and matrix, grain refinement,
and strain hardening were considered as the strengthening mechanisms in the manufactured composites.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction Many potential applications of MMCs prompted the present

authors to invent and propose another solid state process named
Metal matrix composites (MMCs) are widely used in aerospace, accumulative press bonding (APB) for manufacturing MMCs. Up
military, and automotive industries due to their excellent proper- to now, tungsten carbide (WC) is the only particle dispersed in
ties such as high ratio of strength/density, improved elastic modu- the surface layer of metals such as aluminum and, consequently,
lus and high wear resistance [1,2]. There are several traditional the resultant hard coatings improves the wear properties of matrix
processing routes to prepare MMCs such as casting, powder metal- [17–19]. The conventional processes are rarely used for producing
lurgy and spray forming [3,4]. Each of these processes has its own bulk Al/WCp composites because the density and melting point of
drawbacks such as non-uniform distribution of the reinforcement, WC (15.63 g/cm3, 3143 K) is significantly higher than those of alu-
poor adhesion between the matrix and the reinforcement, and minum (2.70 g/cm3, 930 K) [19]. The objective of the present study
undesirable chemical reaction [5–7]. Recently, accumulative roll is to produce bulk nanostructured Al/10 vol.% WC particulate com-
bonding (ARB) has been introduced as a new solid state method posite using APB process. Furthermore, the effect of number of APB
to produce particle reinforced MMCs without the above mentioned cycles on the microstructure and mechanical properties of mono-
problems [8,9]. Up to now, several MMCs including Al/Al2O3 [2], Al/ lithic aluminum and Al/WCp composite were examined.
SiC [10,11], Al/B4C [12], Cu/Al2O3 [8], Al/CNT [13], Al/Cup [14], Mg/
CNT [15] and Al/Wp [16] have been fabricated by ARB process. 2. Experimental procedure

2.1. Materials
⇑ Corresponding author. Tel.: +98 21 64542966; fax: +98 21 66405846.
E-mail addresses: [email protected], [email protected] (S. Amir- As-received commercial AA1050 aluminum strips with the
khanlou), [email protected] (M. Ketabchi). dimensions of 100 mm  50 mm  1.5 mm were annealed at

0261-3069/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2013.04.032
368 S. Amirkhanlou et al. / Materials and Design 51 (2013) 367–374

623 K in ambient atmosphere for 1 h, and WC powder with average

particle size of about 10 lm, were used as raw materials. The
chemical composition of aluminum strips and the micrograph of
WCp powder used in present study are demonstrated in Table 1
and Fig. 1, respectively.

2.2. Surface preparation

To create a satisfactory metallurgical bond by press bonding, it

is essential to remove any contamination that may be present on
the surface of the aluminum strips. The aluminum surfaces usually
contains humidity, dust particles, greases, adsorbed ions, and alu-
mina oxide. Several authors [20–22] have noted that the best
method for achieving high mechanical bonding quality between
strips is degreasing surface followed by scratch brushing. Along
Fig. 1. Typical SEM image of the used WCp powder.
these lines, the strips were degreased with acetone bath and, sub-
sequently, scratch brushed by a steel crimped wire wheel brush
attachment (with 0.4 mm wire diameter) mounted in the drill ma- 2.4. Microstructural evaluations
chine (AEG SBE 600R) with peripheral speed of 2800 rpm. The ini-
tial surface roughness of the specimens was 0.6 lm, which after Scanning electron microscopy (SEM, Philips XL30) was em-
scratch brushing rose to about 5.5 lm. Surface roughness was ployed to examine the distribution of WC particles through the dif-
measured by the SM7 roughness profile meter apparatus and ferent cycles of APB process. The X-ray pattern of the
according to ASTM D7127 – 05 standard. To avoid contamination manufactured Al/WCp composite was recorded with an X-ray dif-
and thick alumina layers formation, the press bonding process fractometer (XRD). The result was used for the microstructural
must be carried out immediately after degreasing and scratch characterization. The XRD experiment was conducted on the spec-
brushing. imen with dimensions of 10 mm  10 mm  1.5 mm by a Philips
X’PERT MPD X-ray diffractometer with Cu Ka radiation in the
range of 2h ¼ 25—95 using a step size of 0.05° and a counting time
2.3. Manufacturing of Al/WCp composite by APB process of 1 s per step. Consequently, XRD pattern was analyzed by using
X’PertHighScore software, and microstructural phases of the com-
Fig. 2 illustrates the schematic of APB process for producing posite were characterized. The crystallite size of the specimen was
Al/10 vol.% WCp composite. This process was performed in two calculated from the XRD patterns applying the Williamson–Hall
steps. To achieve a good dispersion of WC particles between method [23].
strips, an acetone-base suspension was prepared and put under
ultrasonic waves with frequency of 48 kHz for 30 min. After sur- kk
b cos h ¼ þ 2Ae sin h ð1Þ
face preparation, ultrasonicated WC powder in acetone was d
sprayed between the two aluminum strips with an atomizer.
where h is the Bragg diffraction angle, d is the crystallite size, e is the
Then, WC particles deposited and acetone evaporated in air, so
average internal strain, k is the wavelength of X-ray (0.154056 nm
that the brushed surface of one strip uniformly covered with
for Cu Ka radiation), b is the diffraction peak width at half maxi-
WC particles. The amount of WCp powder, dispersed on the sur-
mum intensity, k is the Sherrer constant (0.91), and A is a coeffi-
face, was 2 vol.% per cycle. Then, the two strips were put on each
cient, depending on the distribution of strain, which is near to
other and stacked. The stack strips were carefully handled to
unity for dislocations. In this method, bcos h is plotted versus sinh
avoid renewed contamination. The cold press bonding process
and the intercept of the linear extrapolation yields to the crystallite
was performed on the stacked strips with no lubrication, employ-
size.
ing a laboratory hydraulic press machine (Toni Technik Bau-
stoffprüf systeme GmbH), with a loading capacity of 200 tons.
The press bonding process was carried out with a specific amount 2.5. Mechanical properties
of reduction equal to 50%. Then, the press bonded strips were cut
in half. The same procedure was repeated up to five cycles in the The tensile test specimens were machined from the APBed
first step (Fig. 2a). First step of APB process was designed for add- strips, according to the ASTM E8/E8M standard. The gauge width
ing reinforcement into metal matrix and thereby producing MMC. and length of the tensile test specimens were 6 ± 0.1 and
In the second step (Fig. 2b), the mentioned procedure was re- 25 ± 0.1 mm, respectively. The tensile test was carried out at a
peated again up to 14 cycles without adding WCp powder. Second nominal strain rate of 1.6  101 s1 by a Houndsfield H50KS ma-
step was designed for dispersing reinforcement particles in all chine. The total elongation of specimens was measured from the
part of the matrix. The same process was employed for the pro- difference in the gauge length before and after testing. To have
duction of the monolithic aluminum, while the aluminum strips accurate results, three tensile experiments were conducted on each
were APBed without adding WCp powder in any steps of APB specimen and subsequently averaged.
process.
3. Results and discussion

Table 1 3.1. SEM observation

Chemical composition of the used AA1050 aluminum strip.

Element Al Si Fe Mn Cu Mg Zn Ti Other The microstructure variations of Al/WCp composites produced

by different cycles of APB process in two different magnifications
wt.% 99.50 0.20 0.22 0.02 0.01 0.01 0.01 0.01 0.02
are shown in Fig. 3. It can be seen from Fig. 3a that in the primary
 S. Amirkhanlou et al. / Materials and Design 51 (2013) 367–374 369

Fig. 2. Scheme illustrating procedure to fabricate Al/WCp composite strip through APB process; (a) first step: adding WC particles between the strips, (b) second step:
removing discontinuities between the layers and distributing WC particles in all part of aluminum matrix.

cycle of APB process, the specimen consists of a narrow layer of WC to the cluster–matrix interface, are less constrained than those in
particles and a wide zones which are particle free. The length of the interior of the clusters. Therefore, these particles flow by tum-
particle free zones reaches 750 lm across the thickness of the bling along the interface of the clusters as a result of the aluminum
strip. It is also obvious that there is some porosity inside WCp clus- matrix shearing effect. By increasing the imposed strain, the clus-
ters and between aluminum layers. The entrapped air inside the ters continue changing their size and shape, as more particles are
agglomerated particles, coupled with the hindered metal flow by removed from the cluster surfaces and are transported to the end
the mentioned particles, contributes to the formation of porosity of the elongated clusters. By continuing deformation, the clusters
[24,25]. After two cycles (Fig. 3b), there are still very large particle show a preferred orientation, string themselves out perpendicular
free zones (375 lm), and big cluster of particles. However, the to the press direction and, finally, particles are uniformly dispersed
porosity between the WC particles and also among the aluminum in the matrix. In fact, the flow of aluminum matrix is the main rea-
layers noticeably decreases in this stage. As it can be seen from son causing the WC clusters to be broken and the particles to be
Fig. 3c, after three cycles, the composite contains seven layers of separated from each other. As a result, the particles distribute more
WC particles and the length of particle free zones is reduced to uniformly throughout the aluminum matrix. In summary, by
187.5 lm. After seven and 10 cycles (Fig. 3d and e) the composite increasing the number of APB cycles the following positive results
should be contain of 127 and 1023 WCp layers, respectively. How- are obtained through the production of Al/WCp composite: (a) the
ever, as the interface between different layers is not identifiable uniformity of WC particles in the aluminum matrix improves, (b)
anymore, it is very difficult to recognize the number of layers in the porosity of composite is eliminated, (c) the particle free zones
the micrographs. It is seen that in the second step of APB process, decrease, and (d) the cluster characteristics are enhanced.
the laminate structure including aluminum and WCp layers com-
pletely vanishes and changes to a particle-reinforced composite. 3.2. X-ray diffraction analysis
In fact, WC particles distribute in all part of aluminum matrix,
and the length of particle free zones reaches to less than The XRD pattern and Williamson–Hall plot of the 14 cycles
50 lm. However, the high magnification micrographs of these APBed composite are shown in Fig. 4. The Williamson–Hall method
composites show that there are still some clusters in the composite was used to calculate crystallite size from the XRD pattern of the
microstructures. After the 14th cycle of APB process, the clusters produced MMC. As it can be seen from Fig. 4a, the diffractions of
and particle free zones are almost disappeared, and the composite the four crystallite planes ((1 1 1), (2 0 0), (2 2 0) and (3 1 1)) are
contains a completely uniform distribution of WC particles. The more intensive the rest ones in the aluminum matrix. Therefore,
clusters characteristics consist of the cluster shape, the particle the diffractions of these four peaks are considered to estimate
volume fraction in the cluster, and the volume fraction of clusters the crystallite size of the composite. From the intercept of the Wil-
in the matrix [26–28]. If the sphericity of the cluster shape in- liamson–Hall plot (Fig. 4b), the calculated mean crystallite size is
creases, the particle volume fraction in the clusters decreases, 58.4 nm (0.91  0.154056 nm/0.0024 = 58.4 nm). That is, the 14th
and the volume fraction of clusters in the matrix decreases, the cycles of APB process successfully developed a nanostructured
manufactured composite would have better mechanical properties Al/WCp MMC. Although Williamson–Hall method has many appli-
[3,29]. According to Fig. 3, when the number of APB cycles in- cation in nano-technology including characterization of powders
creases, the aforementioned cluster characteristics are improved and deformed polycrystalline metals, some researcher reported
and, consequently, these characteristics of the specimen processed that the grain size measured by XRD (using Williamson–Hall meth-
by 14 APB cycles modifies absolutely. In other words, by increasing ods) is somewhat smaller compared to TEM (transmission electron
the number of APB cycles, the WC particles in the clusters are dis- microscopy) observations [27]. The mechanism of the nanostruc-
persed from the interfaces to all part of the aluminum matrix, and ture formation during APB process is an important issue, and needs
the distribution of WC particles in the matrix improves. A number further supplementary investigations. However, the present
of mechanisms contribute to the removal of the lamination struc- authors propose four probable mechanisms as follow: (a) continu-
ture and the dispersion of WC particles. At the initial cycles of the ous recrystallization: recent experiments [30,31] suggest that the
APB process, WCp layer breaks up to the large clusters during press formation mechanism of nano/ultra-fine grains in severe deformed
deformation and, subsequently, the aluminum matrix extrudes metals is continuous recrystallization (or in situ recrystallization)
into the clusters. As the deformation of the hard WCp clusters is characterized by ultra-fine grain subdivision, creation of clear
noticeably less than the soft aluminum matrix, the matrix flows sub-boundaries by recovery, and short-range grain boundary
past the clusters, causing shear flow. The WC particles, adjacent migration. It has been reported [31,32] that the continuous
370 S. Amirkhanlou et al. / Materials and Design 51 (2013) 367–374

Fig. 3. Typical SEM micrographs of the Al/WCp composites produced by the APB process in various cycles and magnifications: (a) first, (b) second, (c) third, (d) seventh, (e)
10th and (f) 14th cycles.
 S. Amirkhanlou et al. / Materials and Design 51 (2013) 367–374 371

Fig. 4. XRD pattern (a) and Williamson–Hall plot, (b) of the Al/10 vol.% WCp composite processed by 14 APB cycles.

changes in misorientation are converted into the high angle Fig. 4a also illustrates that the manufactured Al/WCp composite
boundaries by rearrangement of the geometrically necessary dislo- consists of only aluminum and WC phases, and no effect of Al4C3,
cations through short range diffusion. The short range diffusion is W2C, and Al–W intermetallic exists. Generally, to fabricate high
possible even at ambient temperature due to the temperature in- quality particle-reinforced MMCs with desirable mechanical prop-
crease caused by plastic deformation [32–34]; (b) severe shear erties, several important factors are required [39–41]: (a) good dis-
deformation: The severe shear strain resulted by friction between tribution of reinforcement in the matrix without particle free zones
the strips and the press under dry condition can be counted as an- and clusters, (b) perfect bonding between reinforcement and ma-
other important reason for grain refinement. This shear deforma- trix without any undesirable reactions between them, and (c) lack
tion significantly increases the equivalent strain and promotes of porosity in the created composite. According to the microstruc-
grain refinement [35,36]; (c) pinning of the dislocations by WC tural observations of the present investigation (Figs. 3 and 4), APB
particles: By performing 14 cycles of APB process, a uniform distri- process is an applicable method to produce highly uniform MMC
bution of WC particles is obtained in aluminum matrix. The WC without any noticeable porosity and undesirable phases.
particles can be considered as the obstacles to the dislocation mo-
tions and also the dislocations accumulation. High dislocations 3.3. Mechanical properties
density causes the higher rate of diffusion. Hence, the sub-grain
boundaries (formed by rearrangements of the dislocations) further The variations of the tensile strength and the elongation of Al/
evolve into grain boundaries with large angle of misorientation, WCp composite and monolithic aluminum versus the number of
and therefore the grain refinement facilitates [37]; (d) formation APB cycles are shown in Figs. 5 and 6, respectively. It can be seen
of nano-layer structure: After 14 cycles of APB process the thick- from Fig. 5 that by increasing the number of APB cycles, the tensile
ness of aluminum matrix layers reaches to 91.5 nm (thickness of strength of the both aluminum and Al/WCp composite improves. It
strip/number of layers = 1500 lm/214 = 91.5 nm). According to has been widely reported [32,33,35] that strength variations in se-
the literature [38], interfaces of these layers can be treated as the verely deformed materials are governed by two main strengthen-
strong barriers against moving dislocations, accumulating disloca- ing mechanisms: Grain refinement and strain hardening by
tions. Finally, it refines the crystallite size same as WC particles. dislocations. Strain hardening (or dislocation strengthening) plays
372 S. Amirkhanlou et al. / Materials and Design 51 (2013) 367–374

an important role in enhancement of the strength in the initial

stages of severely deformed metal processes, while at final stages
higher strength is achieved by grain refinement [28,32]. Since both
the materials in the present investigation (monolithic aluminum
and Al/WCp composite) have been produced by the same process
(APB technique), the two mentioned mechanisms exist during
the deformation of the both materials. However, in regards of the
composite material, there are some extra strengthening mecha-
nisms due to the presence of the WC particles: (a) uniformity of
the WC particles distribution: by increasing the number of APB cy-
cles, the WC particles in the aluminum matrix are dispersed more
uniformly (Fig. 3). Hence, the distance between the Al/WCp inter-
faces increases, and during plastic deformation the cracks initiated
in the interfaces will propagate and link up with other cracks later.
Thus, the tensile strength and the elongation of Al/WCp composite
improve; (b) strengthening role of the WC particles: WC particles
can increase the threshold stress for dislocation glide and cause
the generation of additional dislocation around the WC particles
[27], decreasing the mobility of dislocations during plastic defor-
mation. This effect leads to increase in the strength and decrease
Fig. 6. The elongation of the monolithic aluminum and the Al/WCp composite
in the elongation of APBed Al/WCp composite. During plastic defor- produced by the APB process versus number of cycles.
mation, Al/WC interfaces are the suitable sites for initiation and
propagation of cracks. In addition, it is well known that higher vol-
ume fraction of particles results in more strain hardening during of porosity in MMCs results in a lower tensile strength and elonga-
plastic deformation. Hence, the tensile strength enhances while tion [25]. When the number of APB cycles increases, the porosity
the elongation lessens [2,8]; (c) coefficients of thermal expansion across the specimens decreases due to the good formability of
(CTE): the specimen temperature increases during plastic deforma- the aluminum matrix and press pressure (Fig. 3). Thus, tensile
tion [27]. On the other hand, the CTE of WC and aluminum are strength and elongation enhances.
6  106 K1 and 23  106 K1, respectively [6]. Therefore, while As it can be seen in Fig. 5, the tensile strength of the final MMC
the strips is cooling between the APB cycles, WC particles and alu- (216 MPa) is 2.45 and 1.2 times higher than those obtained for an-
minum matrix generate dislocations in the specimen as a result of nealed (88 MPa) and APBed monolithic aluminum (180 MPa),
multidirectional thermal stress at the Al/WCp interfaces, induced respectively. This can be related to the extra strengthening mech-
by the large CTE difference between the matrix and the reinforce- anisms existed in MMC compared to the both annealed and APBed
ment. Thus, the tensile strength improves and the elongation de- pure aluminum strips. The elongation values of the Al/WCp MMC
creases; (d) bonding quality of Al/WCp interfaces: in MMCs the and monolithic aluminum produced by the APB process versus
fracture mechanism is dominated by the cracks which initiate at the number of cycles are shown in Fig. 6. Like the other severely
the interface and propagate through the interface and links up with deformed metal processes, such as ARB and equal channel angular
the other cracks or matrix/reinforcement interface, resulting in pressing (ECAP), elongation values of the monolithic aluminum
failure. When the number of APB cycles increases, the bonding be- and Al/WC composite lessens in the first cycle of the process due
tween the WC particles and the aluminum matrix becomes stron- to the reduction of dislocations mobility and the small number of
ger due to the greater pressure of the applied press, enhancing the shear bands [28,32,42]. Furthermore, according to Fig. 6, the elon-
tensile strength and elongation values; (e) porosity: the presence gation of MMCs strip is lower than that of monolithic aluminum in
each APB cycle. This matter is attributed to the presence of Al/WCp
interfaces which act as a crack source or propagation route during
the tensile test. At the first step of APB process, when the number
of cycles increases, the elongation of MMC strips decreases in con-
trast to the monolithic aluminum curve. This can be related to the
strengthening role of WC particles, uniformity, and bonding fac-
tors. That is, at the first step of APB process, when the number of
cycle increases, the intensifying role enhances (due to the increase
in the alumina volume fraction), and the uniformity and bonding
quality decreases. Totally, all of these changes reduce the elonga-
tion value. Elongation values at the end of the first step (fifth cycle
of APB process) for monolithic aluminum and Al/WCp composite
are 9.3% and 3.6%, respectively. However, the mentioned values
at the end of the second step (14th cycle of APB process) reach
to 10.2% and 6.4%, respectively. Although the second step of APB
process improves the elongation of the monolithic aluminum by
9.7%, it is worthy to note that this step greatly enhances the elon-
gation of the MMC by 78%. This noticeable enhancement can be
attributed to the improvement of the uniformity and the bonding
quality factors at the second step for MMC. The results of the pres-
ent investigation, particularly those which are illustrated in Figs. 3
and 6, show that the second step of APB process is suitably de-
Fig. 5. The tensile strength of the monolithic aluminum and the Al/WCp composite signed to obtain a uniform distribution of WC particles in through-
produced by the APB process versus number of cycles. out the aluminum matrix, to improve bonding quality of the
 S. Amirkhanlou et al. / Materials and Design 51 (2013) 367–374 373

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