Materials and Design 30 (2009) 2911–2918

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Materials and Design

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

High-strength, high-conductivity ultra-fine grains commercial pure copper

produced by ARB process
Sayed Abdollah Hosseini, Habib Danesh Manesh *
Dept. of Materials Science and Engineering, School of Engineering, Shiraz University, Zand Ave., Shiraz, Fars, Iran

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

Article history: Accumulative roll-bonding process is a severe plastic deformation process capable of developing grains
Received 28 October 2008 below 1 lm in diameter. In this study, microstructure, mechanical properties and electrical conductivity
Accepted 12 January 2009 of commercial pure copper strips processed by accumulative roll-bonding were investigated. Transmis-
Available online 20 January 2009
sion electron microscopic micrographs of the strips produced by eight cycles of accumulative roll-bond-
ing process showed ultra-fine grains 180 nm in size with high angle grain boundaries. Also tensile
Keywords: strength and microhardness of the accumulative roll-bonding processed samples increased with increas-
A. Non-ferrous metals and alloys
ing the number of accumulative roll-bonding cycles. Whereas, the elongation dropped abruptly at the
D. Bonding
E. Electrical properties
first cycles, above which it increased slightly. The electrical conductivity decreased with increasing accu-
mulative roll-bonding cycles up to 6 cycles and then increased up to 8 cycles of accumulative roll-bond-
ing process.
Ó 2009 Elsevier Ltd. All rights reserved.

1. Introduction material to be produced is not limited [8]. Only ARB is appropriate

According to the fast developments in electronic industries,
there is a great, unprecedented demand for high-strength, high-
conductivity materials. The highly alloyed Cu is the most widely
used material in this respect. Since in alloyed Cu, alloying elements
play role as impurities, electrical conductivity of these materials is
inherently lower than unalloyed counterpart, in a way that the
electrical conductivity values for the commercially available
high-strength connective materials are, only in the range of 10–
15% IACS (International Annealed Copper Standard) [1]. To resolve
this problem ultra-fine grains (UFG) or nano structure commercial
pure copper, with no alloying elements added can be used. This
goal can be obtained by some kind of sever plastic deformation
(SPD) processes. SPD can be explained as deformation to large
strains below recrystallization temperature without intermediate
thermal treatments that can result in UFG structures [2]. Several
noble techniques have been developed to create the high strain
in metals with minimal changes in the initial sample dimensions,
such as equal-channel angular pressing (ECAP) [3,4], high-pressure
torsion (HPT) [4,5], multi axial forging (MAF) [6], constrained
groove pressing (CGP) [7], and accumulative roll-bonding (ARB)
[2,8–10]. Among these processes, the ARB process developed by
Saito et al. [8], has several advantages over other SPD process such
as (1) forming facilities with large load capacity and expensive dies
are not needed, (2) high productivity rate, and (3) the amount of
to manufacture nanocrystalline and ultra-fine grained sheets and
plates, which are the most widely used material shape in the com-
mercial and industrial fields, due to its feasibility as a continuous
process. The ARB process includes roll-bonding of cleaned and
stacked sheets by 50% thickness reduction, cutting them into
stacks and then roll-bonding again. By repeating this procedure,
very high strains have been introduced successfully into materials,
and significant structural refinement has been achieved [2,8,9].
In this study ultra-fine grained commercial pure copper strip
produced by ARB process and then the microstructure, mechanical
properties and electrical conductivity of ARBed samples were
investigated.
2. Experimental procedure
2.1. Materials
Commercial pure copper strips with the specifications shown in
Table 1 were used in this study. About 300 mm long, 30 mm wide,
and 1 mm thick fully annealed copper strips were prepared to en-
sure consistent specimen hardness with an equiaxed grains with
the mean grain size of 17 lm. Optical micrograph of the initial
sheets is shown in Fig. 1.
2.2. ARB process

* Corresponding author. Tel.: +98 711 230 7293; fax: +98 711 230 7293. In the ARB process, the sheets were scratch-brushed (circular
E-mail address: daneshma@shirazu.ac.ir (H.D. Manesh). steel brush with 0.35 mm diameter wire and surface speed of

0261-3069/$ - see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2009.01.012
2912 S.A. Hosseini, H.D. Manesh / Materials and Design 30 (2009) 2911–2918

Table 1
Specification of initial copper strips.

Material Chemical Temper Tensile Elongation Hardness

composition (mass%) strength (%) (HV)
(MPa)
Commercial 98.51Cu, 0.767Zn, O 251.9 50.42 81.9
pure 0.139Fe, 0.472Pb,
copper 0.0541Co, 0.016Sn,
0.013Cd, 0.0064Mn,
and 0.0046Cr

Fig. 3. Schematic illustration of the principle of electrical conductivity measure-

ments by four-point-probe technique.

optical investigations were carried out at the cross sections which

were normal to the rolling direction.

2.4. Microstructure evaluations

The microstructure evaluations of the copper sheets ARBed by

various cycles were carried out by transmission electron micro-
scope (TEM). Transmission electron microscopic micrographs and
the corresponding selected area diffraction (SAD) patterns were
obtained by utilizing a Philips-CM200 operating at 200 kV. Thin
foils parallel to the rolling plane (Rolling Direction–Transverse
Direction or RD–TD plane) and 350 lm below the surface were
prepared using a jet thinning method in 200 ml CH3OH + 100 ml
HNO3 solution at 30 °C.

Fig. 1. Optical micrograph of commercial pure copper used in this study, 400. 2.5. Mechanical properties

2.5.1. Tensile properties

13.5 m s1) to remove surface oxides and rinsed with acetone
The tensile specimens were machined from the rolled sheets
(with two steps) to degrease. After these surface preparations
according to the 1/5 scale of the JIS-No. 5 specimen, oriented along
two sheets were stacked and bound tightly. Then the stacked
the rolling direction. The gauge length and the width of the tensile
sheets were rolled to 50% reduction in thickness. The roll-bonded
specimens were 10 and 5 mm, respectively. Tensile test at ambient
sheet was cut in half and stacked to the initial thickness. The
temperature was carried out at a nominal strain rate of
stacked sheets were rolled again with the same reduction ratio
8.3  104 s1 by using an instron universal testing machine. Total
and the same procedure was repeated up to eight cycles (the total
elongation of the specimens was measured from the difference in
equivalent strain was 6.4) at ambient temperature. Fig. 2 illustrates
the gauge length before and after testing.
ARB process principles. The number of interfaces would be 2n1.
Roll bonding was carried out without any lubricant by the use of
2.6. Microhardness
two mills having a roll diameter of 136 mm. The roll peripheral
speed was 5.55 m min1, so that the mean strain rate during the
Vickers microhardness (HV) test, using a load of 25 g for 15 s,
roll-bonding would be 5.5 s1.
was performed on the cross section RD–ND plane and through
the thickness of the ARB-processed samples. Mean value of 10 sep-
2.3. Evaluation of cold roll-bonding process
arated measurements taken at randomly selected points was
reported.
Bonding condition between layers of ARBed copper sheets
through various passes evaluated by the optical micrographs. All
2.7. Electrical conductivity

A digital apparatus with maximum tolerance of 1 nX was

implemented for the measurements via four-point-probe method.
Tungsten probes were selected to generate electrical connection.
According to Fig. 3, electrical current (I) was imposed by the two
outer probes on the samples after which the potential difference
caused between two points of a specific span was measured by
the apparatus. Based on these measurements, the device reports
the electrical resistance of materials with maximum tolerance of
1 nX. Smith [11] has proposed some formulas for the four-point-
probe method, relating material’s resistivity with electrical resis-
tance and the geometry of samples. Resistivity can then be calcu-
lated by:
V
q ¼ G  ¼ G  R; ð1Þ
Fig. 2. Schematic illustration of the principle of ARB process. I
 S.A. Hosseini, H.D. Manesh / Materials and Design 30 (2009) 2911–2918 2913

where q and R, are the resistivity and the measured electrical resis-
tance of the sample respectively. G, the correction factor will in turn
be calculated by:
 
P b a
G¼  t  R1 ; ; ð2Þ
ln 2 s b
where lnP2 is a coefficient due to a geometrical factor, t is sample
thickness, and R1 is a correction factor due to the rectangular shape
of the sample expressed as a function of sample’s length by Smith
(a), sample’s width (b), and the distance between two adjacent
probes (s).

3. Result and discussion

3.1. Cold roll-bonding mechanisms of copper sheets

In the present work, the degreased and scratch-brushed sur-

faces were investigated to make an assessment of the dominant
mechanisms of cold roll welds produced between the strips. Fig. 5. Optical micrograph of the surface of the layer that has peeled and had
Fig. 4 shows the microscopic image of prepared surfaces. As it previously rolled by 50% reduction in thickness: (a) 400 (b) 1000.
seems, scratch brushing causes grooves and depressions due to dis-
placement of material on the surface and also material ripped off
cracks and virgin metal will be resulted, and thereof, the stronger
from surface. In other words, scratch brushing produces a thin sur-
cold weld will be achieved [13,16].
face layer which is severely deformed and hardened [12–15]. This
Paying attention to these results, the process of producing cold
layer acts as a thin brittle cover on the surface. Due to the fact that
roll welding of copper strips caused by former degreasing and
oxides are colonized on metal surface with weak bonds, it is neces-
scratch brushing can be considered as the following stages:
sary to remove oxides to produce strong bonds [16]. Scratch brush-
ing is a process to get rid of surface oxides in addition to producing
(I) Continuous breaking of the brittle surface layers as a result
a thin hardened layer as mentioned previously. It is important to
of deformations caused by rolling and generating surface
note that oxides are formed rapidly, so they might be rebuilt before
cracks.
the rolling process. So the time gap between scratch brushing and
(II) Extrusion of sublayer metals through the cracks under the
rolling is crucial and should be kept minimum [17]. This time was
roll pressures.
arranged to be less than 120 s.
(III) Virgin metals of opposite layers getting as close as atomic
Fig. 5 shows the surface of the layer which has been peeled after
distances. And finally generating metallic bonds.
being rolled by 50% reduction in thickness. As it is seen, the brittle
cover layers produced by scratch brushing are crushed via passing
Fig. 6 schematically shows these stages called surface film the-
through the rolls and bearing a continuous deformation from the
ory [18,19]. This theory is promising only when: (a) the contact of
entrance to the rolls gap till it gets out. Along with the crushing
the stacked stripes includes hardened and brittle layers and (b)
of these layers, some cracks will be generated perpendicular to
limited relative motion between layers [13,16–18].
the rolling direction. Sublayer metal will emerge through these
cracks which are called virgin metals. Virgin metals will be in con-
3.2. The bonds generated between layers during ARB process
tact with these from the other layer and the cold weld of layers
provided by the virgin metals along together [16]. In other words,
Fig. 7 shows the RD–ND planes of the ARBed commercial pure
the more deformation amount of the layers, the more surface
copper strips after one, two, four and eight cycles. The last interface
(indicated by the arrows in Fig. 7) introduced in every cycle was
partly observed only by etching. This indicates that the bonding
of the interface was quite well by 50% thickness reduction. After
ARB cycles, the interfaces are almost invisible, except the last
one (Fig. 7b–d). For example, after 8 ARB cycles (Fig. 7d), (28  1)
interfaces are produced [20]. However, only a few unbonded parts

Fig. 4. Degreased and scratch-brushed surface of commercially pure copper, 400. Fig. 6. Schematic illustration of three stage of surface film theory.
2914 S.A. Hosseini, H.D. Manesh / Materials and Design 30 (2009) 2911–2918
Fig. 7. Optical micrographs of commercial pure copper after ARB process, (a) one, (b) two, (c) four and (d) eight cycles, 400 (last interfaces indicated by arrows).
of interface can be seen in the specimens. This means that the sub-
sequent cold roll-bonding sufficiently improved the bonding of
interface introduced in a previous cycle. In other words, the cold
roll-bonding process was attained by the ARB process.
3.3. Microstructure evaluation
TEM microstructure and corresponding SAD patterns observed
at rolling plane of the ARB-processed specimens after four, six
and eight cycles are shown in Fig. 8. After four cycles (Fig. 8a),
the SAD pattern showed a net pattern, indicating an area with
low misorientation. Therefore, the grain structure at this stage in-
cluded mainly subgrains or dislocation cell structures. The dislo-
cation density was relatively low inside the cells. After four
cycles, microstructure showed a mixture of deformed and non-
deformed grains with some dislocation tangles (Fig. 8a). This
was predictable because plastic deformation is inherently an
inhomogeneous process at microscopic level. It showed that rela-
tively coarse dislocation cells formed by the first pass defined by
operation of multi-directional slip [21,22]. For the specimen after
six cycles (Fig. 8b), dislocation density increased, while, compared
to Fig. 8a, density in cells decreased and the cell size became fi-
ner. The ultra-fine grained structure became more dominant
and some regions showed scattered diffraction patterns shown
in Fig. 8b, which is an indication of large misorientation. The
grain structure of specimen at this stage included subgrain di-
vided by dislocation walls. It should be emphasized that the for-
mation of the ultra-fine grains is regionally heterogeneous in the
highly strained materials [10]. The fraction of the ultra-fine
grained regions increased with increasing the number of ARB cy-
cles, i.e. strain. The specimen, after eight cycles (Fig. 8c), was
filled with the ultra-fine grains with average grain size of
180 nm, homogenously distributed. Fig. 8c shows the ultra-fine
grains in which the dislocation density is very low inside, and
are surrounded by strongly deformed boundaries, which have a
high density of dislocations. This is quite different from the spec-
imen after four ARB cycles (Fig. 8a).
From Fig. 8, a sequence of grain refinement by accumulative
roll-bonding (ARB) process can be deduced. In the ARB process of
this work the evolution of microstructure in the RD–TD plane
evolved in the following way with number of cycles (or equivalent
strain): (1) the creation of a fine dislocation cell structure or sub-
grain network with low angle grain boundaries, (2) the refinement
of dislocation cells or subgrains due to operation of multi-direc-
tional slip, (3) an increase in the misorientation of the early low an-
gle boundaries, and (4) a well-defined grain structure with sharp
high angle boundaries [10,21,23,24].
The mechanism of the UFGs formation during SPD is still an is-
sue under discussion. However, recent investigations suggested
that the formation process of the UFGs is continuous recrystalliza-
tion (or in situ recrystallization) characterized by ultra-fine grain
subdivision, recovery to form clear boundaries, and short-range
grain boundary migration [20]. It was reported that the continuous
change in misorientation are converted into the planner bound-
aries (or high angle boundaries) by rearrangement of the geomet-
rically necessary dislocations by short-range diffusion. The short-
range diffusion is possible even at ambient temperature due to
the temperature rise by plastic work [25].
 S.A. Hosseini, H.D. Manesh / Materials and Design 30 (2009) 2911–2918 2915

Fig. 8. TEM micrograph and corresponding SAD patterns of commercial pure copper after RT-ARB process, (a) 4 cycles, 38kx, (b) 6 cycles, 99kx and (c) 8 cycles,115kx.

The redundant shear strain due to friction between the rolls and
the specimen plays an important role in grain refinement by ARB
process [20,26–28]. The role of redundant shear strain in grain
refinement was considered from viewpoints of equivalent strain,
strain gradient and strain path [26–28].
3.4. Mechanical properties
The tensile strength and elongation (total elongation) obtained
from the engineering stress–strain curves of copper sheets are pre-
sented in Fig. 9 as a function of ARB cycles. The tensile strength
greatly increased by two ARB cycles, and then increased with
increasing strain. The tensile strength reached 723.56 MPa after
eight cycles, which is 2.87 times larger than that of the starting
sheet (251.9 MPa). On the other hand, the total elongation de-
creased down to 9.81% by one ARB cycle and then increased
slightly, and reached to 16% after eight cycles. The strengthening
in ARB-processed commercial pure copper may be attributed to
strain hardening or dislocation strengthening (rp) and grain refine-
ment hardening or boundary strengthening (rb) [27–29]. rp is cal-
culated based on the assumption of dislocation hardening, i.e.
rpaq1/2; rb is calculated based on the assumption of Hall–Petch
strengthening, i.e. rbad1/2 where d is the distance between
impenetrable boundaries [29,30]. Up to three cycles, strain harden-
ing or dislocation strengthening play a main role in the strength in-
crease, and the formation of submicron subgrains or dislocation
cells also contribute to the strength [30]. From four cycles, the
strength increasing was most due to the evolution of the grain
structure and formation of UFGs. Strain hardening has less and less
effect. The number of UFGs with high angle grain boundaries in-
creased with increasing the ARB cycles up to eight cycles. It should
be noted that introduction of a hard surface layer on the strips due
to wire brushing is one possibility to improve the strength [30].
Furthermore, the ductility decrease of ARB-processed commercial
2916 S.A. Hosseini, H.D. Manesh / Materials and Design 30 (2009) 2911–2918
Fig. 9. Variation of strength and elongation with respect to accumulative strain in
RT-ARBed samples.
pure copper sheet was mainly influenced by the strain hardening
[31,32]. However, debonding in the interface in the last pass also
plays an important role in the ductility decrease [31]. Tsuji et al.
[32] showed that strain hardening in materials with grain size less
than 1 lm after ARB process becomes rather difficult to occur. The
sudden drop in uniform elongation in ARB-processed Cu sheets, at
which strain hardening become hard to occur, can be explained in
terms of plastic instability [32]. Plastic instability condition (neck-
ing propagation in tensile test) is explained by the following simple
equation known as considered criterion:
dr
r ; ð3Þ
de
where r and e are true stress and true strain, respectively, and ddre
strain hardening rate. For an ultra-fine grained material, its strength
is high and strain hardening rate is low. As a result, plastic instabil-
ity (necking in tensile test) occurs at very early stage of tensile test
in UFG materials, resulting in a limited elongation below a few
percent.
3.5. Microhardness
The Vickers microhardness of commercial pure copper pro-
cessed at different cycles of the accumulative roll-bonding process-
ing is presented in Fig. 10. It shows an immediate increase in
microhardness by a factor of approximately 1.78 at a strain of 0.8
(first cycle), followed by a minor additional increase up to strains
of 1.6 (second cycle) and 3.2 (fourth cycle) for the rolling plane,
and then essentially no change in the microhardness with subse-
quent straining. After eight cycles, microhardness reached to
185.62 HV for the rolling plane.
The rapid increase of microhardness at relatively low strains
seems to be attributed to strain hardening (based on the density
of dislocations and interaction between them) as a result of sub-
grain boundaries/cell wall formation rather than grain refinement
[2], since the grain refinement at larger strains (Fig. 8c) did not
cause much hardness. The hardening behavior showing saturation
at large strains was previously reported in UFG materials fabri-
cated by severe plastic straining [2,31]. This phenomenon occurs
because the materials reached the steady-state density of disloca-
tion. The steady-state density of dislocations is determined by a
dynamic balance between dislocation generation during plastic
deformation, and annihilation in the dynamic recovery process.
The room-temperature dynamic recovery is enhanced in the
Fig. 10. Variation of microhardness with respect to accumulative strain in ARBed
samples.
ultra-fine grains, due to creation of non-equilibrium high energy
and unstable grain boundaries (high angle grain boundaries) [33].
The hardness distributions along the thickness of the ARB-pro-
cessed specimens before and after two, four and eight ARB cycles
are shown in Fig. 11. The hardness of the specimen before the
ARB process shows a constant value. However, specimens after
two and four cycles show inhomogeneous distribution in the thick-
ness direction. They show higher values near the surface and cen-
ter of specimens. The high value of hardness near the center can be
attributed to the presence of oxide particles along the bonding
interface and hard surface layer formed by wire brushing process
[27,25]. The high value of hardness near the surface is caused by
work hardening due to large redundant shear strain induced by
high friction between roll surface and specimen during the ARB
process [20,26,28]. This hardening by the redundant shear strain
near the surface has also an effect on the hardness at the center
of the ARB-processed specimens, except for specimen produced
by one ARB cycle, because the surface of specimen will be put into
the center of specimen in the next cycle. The fact that the number
of bonding lines (interface) also increases exponentially with the
number of ARB cycles (2n1) should be taken into account in inter-
preting these results. For eight cycles of ARB, the specimens have
255 bonding lines set at intervals of about 3.9 lm. Thus, for high
ARB cycles (for example eight ARB cycles), the hardness measure-
ments tend to be constant along the thickness (Fig. 11). It shows
that the average of hardness should be constant with the increase
of the number of ARB cycles as experimentally observed above.
Fig. 11. The hardness distribution along the thickness of the ARBed specimens of
different cycles.
 S.A. Hosseini, H.D. Manesh / Materials and Design 30 (2009) 2911–2918
Fig. 12. Variation of resistivity and electrical conductivity with respect to different
ARB process cycles.
Fig. 13. Comparsion of mechanical properties and electrical conductivity of
commercial pure copper at anneal condition and after 8 cycles of ARB process
with Cu–Zn alloys at different chemical compositions.
3.6. Conductivity of ARBed commercial pure copper
The result of conductivity evaluations are shown in Fig. 12. As
depicted in this figure the conductivity of samples decreases with
increasing the number of ARB passes, or equally the amount of
strain. This is true as far as six passes after which resistivity de-
clines so electrical conductivity increase. This raise of electrical
conductivity is due to elimination of point defects because of the
dynamic recovery happened by the more increase in temperature
of the final passes with respect to increased temperature in initial
passes. In each pass most of the used energy is dissipated via heat
and only a tiny fraction is stored in material. On the other hand of
the scale, in the ultra-fine grains, due to creation of non-equilib-
rium high energy and unstable grain boundaries (high angle grain
boundaries) the low-temperature dynamic recovery is enhanced
[33]. In addition, the more previous cold work stored in material,
the higher the heat produced in next deformation [34]. On the
other hand, as the number of ARB passes increases, hardness and
strength of the work piece will increase significantly. This will in
2917
turn contribute to the temperature raise in the work piece in the
7th and 8th passes of ARB process.
Fig. 13 shows ultimate tensile strength and electrical conductiv-
ity of different Cu–Zn alloys at different chemical compositions
[35]. These quantities are compared with those of ARBed commer-
cial pure copper strip. According to this figure, although ARB pro-
cessing increases the strength of Cu strips, it does not fall
conductivity in spite of what is seen in alloying treatments. So
via ARB process and by producing nano structure commercial pure
copper, we can strengthen the stripes while retaining their electri-
cal conductivity.
4. Conclusions
In this study, the cold roll-bonding mechanisms, the micro-
structure, mechanical properties and conductivity of a commercial
pure copper severely deformed by the ARB process up to 8 cycles
were investigated. The main results are summarized as follows.
The subsequent cold roll-bonding sufficiently improved the
bonding of interface introduced in a previous cycle. In other words,
the cold roll bonding was attained by the ARB process. UFGs micro-
structures were formed in the commercial pure copper highly de-
formed by the ARB process. The UFGs partially formed after four
cycles of ARB, and the number of grains with high angle boundaries
increased with increasing the strain up to eight cycles. After eight
cycles, the whole volume of the material consisted of the UFGs
with high angle grain boundaries.
The strength of the ARB-processed copper increased with
increasing the accumulative strain and reached up to 723.56 MPa
after eight cycles of ARB process. The strengthening in ARBed com-
mercial pure copper may be attributed to strain hardening and
grain refinement hardening. Microhardness increased with
increasing the accumulative strains up to 3.2 and then showed
slightly change with subsequence straining. So microhardness in-
crease was attributed to strain hardening rather than grain refine-
ment hardening.
Via ARB process and by producing nano structure commercial
pure copper, the stripes can be strengthened while their electrical
conductivity retained. So high-strength, high-conductivity com-
mercial pure copper can be obtained.
Acknowledgments
The authors would like to thank the research board of Shiraz
University and industries and mines organization of Fars province
for the financial support and provision of research facilities used in
this work.
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