Materials Science & Engineering A 577 (2013) 4347

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Materials Science & Engineering A

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

Nanograined TiNb microalloy steel achieved by Accumulative Roll

Bonding (ARB) process
A.A. Tohidi n, M. Ketabchi, A. Hasannia
Mining and Metallurgical Engineering Department, Amirkabir University of Technology, Tehran, Iran

ar t ic l e i nf o

a b s t r a c t

Article history:
Received 25 December 2012
Received in revised form
2 April 2013
Accepted 5 April 2013
Available online 12 April 2013

Over the last decade, nanocrystalline and ultra-ne grained (UFG) materials with grain size less than 1 m
have aroused considerable interest due to their superior mechanical properties compared to conventionally grained materials. In this work TiNb microalloy steel was processed by the severe plastic deformation
(SPD) technique called Accumulative Roll Bonding (ARB) in order to produce an ultra-ne grained
microstructure and improve the mechanical properties. After initial preparation to achieve good sheet
bonding, 8 cycles of ARB at 550 1C were successfully performed. Observation of optical microstructure,
scanning electron microscopy (SEM) micrographs, and X-Ray Diffraction (XRD) peak broadening analysis
were used for the characterization of grain structure of the ARB processed sample. The mechanical
attributes after rolling and cooling were examined. It was calculated that metal's yield and tensile strength
increased by 334% and 215% respectively, while the ductility dropped from as-received value of 34% to 2.9%.
Microhardness of the material was studied at room temperature. There was a continuous enhancement of
hardness by increasing the pass number of the ARB process. At the 8th pass, the hardness values increased
by 230%. The rolling process was stopped at 8th cycle when cracking of the edge became pronounced.
& 2013 The Authors. Published by Elsevier B.V. Open access under CC BY-NC-ND license.

Keywords:
Accumulative Roll Bonding
Severe plastic deformation
Nanograin
Microalloy steel

1. Introduction
The main objective of the transportation and especially automotive industry is aimed at weight and fuel reduction, and hence
energy saving. The aim is therefore to reduce overall vehicle body
weight by using lighter materials or thinner metal sheets and
exploiting the material diversity in order to compensate for the
extra weight, while at the same time not compromising on the
strength. Over the last decade nanocrystalline or ultra-ne grained
(UFG) materials with an average grain size below 1 m have
received considerable attention due to their superior mechanical
properties in comparison to the conventionally grained materials.
The ultra-ne grained sheet materials can be effectively produced
by the relatively new process called Accumulative Roll Bonding
(ARB). This process belongs to the group of severe plastic deformation (SPD) techniques, and it was originally developed and
rstly introduced by Saito et al. [14]. Besides the ARB process,
there are a number of methods all belonging to the SPD techniques, which can be used to obtain an UFG microstructure. These
include: Equal Channel Angular Pressing (ECAP) rstly introduced

Corresponding author. Tel./fax: +98 2144717834.

E-mail addresses: atohidi96@gmail.com, tohidi@aut.ac.ir (A.A. Tohidi).

by Segal [5,6], High Pressure Torsion (HPT) rstly investigated by

Bridgman [7], Cyclic ExtrusionCompression (CEC) developed by
Korbel et al. [8], etc. However, the biggest contemporary limitation
of most SPD processes like ECAP is the up-scaling of process for
mass production and commercial application. On the other hand,
the ARB process is an adequate method for practical application
since it can be easily scaled up and adapted to the conventionally
rolling process to produce large scale UFG metal sheets.
So the advantage of this process over other processes is
concerned with overcoming the difculties connected with residual
porosity in the compacted sample, impurity from ball milling,
processing of large scale billets, and the practical application of
the resulting material.

2. Experimental
TiNb microalloy steel was used in the tests. The chemical
composition of this material is given in Table 1. The grain structure
of as-received TiNb microalloy steel, obtained using optical
microscopy, is shown in Fig. 1a, indicating fully equiaxed ferritic
structure with grain sizes of 520 m. The ARB process was
applied to strip with 2 mm
30 mm
200 mm in size. The surfaces were degreased by acetone and prior to roll bonding the wire
was brushed in order to remove the oxide layer. The strips were
stacked on top of each other and pre-warmed to 550 1C for 200 s
in a furnace. Rolling at an elevated temperature is advantageous

0921-5093 & 2013 The Authors. Published by Elsevier B.V. Open access under CC BY-NC-ND license.
http://dx.doi.org/10.1016/j.msea.2013.04.025

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A.A. Tohidi et al. / Materials Science & Engineering A 577 (2013) 4347

Table 1
Chemical analysis of TiNb microalloy steel.
Fe

Si

Mn

Cr

Ni

Mo

Cu

Ti

Al

Sn

Nb

Base

0.07

0.02

0.33

0.008

0.008

0.01

0.02

0.01

0.02

0.005

0.036

0.003

0.02

Fig. 1. Optical microstructure of a) as-received as well as b) one cycle and c) three cycles ARB processed in TiNb microalloy steel.

load. Each reported hardness was an average of at least three separate

measurements taken at random places on the surface of the ARB
processed sheet.

3. Result and discussion

Fig. 2. Schematic illustration showing the ARB process [2].

for jointability and workability, though too high temperature

would cause recrystallization and remove the accumulated strain
[9]. Two pieces of the strips were roll bonded by 50% reduction
(Von Mises equivalent strain: 0.8) in one pass. The metal sheet
deformation takes place predominantly in the rolling direction.
Roll bonding is carried out without any lubricant by the use of a
two-high mill at a velocity of 0.47 m/s (30 rpm, diameter of rolls
was 30 cm). The furnace is located beside the mill so that the
transfer of the strips for rolling caused minimal loss of heat and
the entry temperature may be safely assumed to be very close to
the furnace temperature. During rolling the two metal strips join
together to form a solid body and can once again be halved, wire
brushed and roll bonded. The process can be repeated many
number of times. In this study, the process was repeated for up
to 8 cycles to give an equivalent strain of 6.4. A schematic
illustration of the ARB process is shown in Fig. 2 [2].
After 8 cycles of the ARB process, the number of bonded layers was
256. The microstructure was examined in the RDTD plane (RD and
TD are the rolling and transverse directions, respectively) by optical
microscopy (OM), scanning electron microscopy (SEM) and X-ray
diffraction (XRD) peak broadening analysis. TiNb microalloy steel
samples were etched by Nital solution after polishing. Tensile direction
was parallel to the rolling direction. Tensile tests were carried out at
ambient temperature using an Instron 8502 testing machine (capacity:
30 ton). The gage length and width of the tensile specimens were 25
and 6 mm, respectively (based on ASTM standard E8-00b). Microhardness of the ARB processed specimens was measured by a Vickers
hardness tester with a pyramidal diamond indenter subjected to 50 g

In order to investigate the bond quality of the ARB processed

TiNb microalloy steel strips, optical examination of the 1, 3, 5 and
8 cycles ARB processed samples was conducted. All optical micrographs were observed along the transverse direction of the rolling
sample. As shown in Fig. 3, following the ARB, bonding is generally
good and there was no effective separation between the layers.
This indicates that the bonding of the interface was quite well by
50% thickness reduction.
Fig. 1a presents the OM micrograph of initial microstructure of
the TiNb microalloy steel. The main linear intercept size of larger
and smaller ferrite grains was 5 m and 25 m respectively. The
microstructure after one ARB cycle showed a mixture of deformed
and non-deformed grains and as shown in Fig. 1b, sheared grains
along the rolling direction were clearly deformed. But after three
cycles, the elongated grains were very thin and were difcult to
distinguish by optical microscopy (Fig. 1c). To demonstrate the
effect of deformation condition on the structural development in
TiNb microalloy steel during the ARB process, the SEM analysis
was used as well. As shown in Fig. 4, at the initial passes of
process, grain renement was not uniform, and the structure
consists of coarse grains adjacent to ne ones; after 3 cycles the
grains show an irregular morphology due to deformation (Fig. 4b
and c); further rolling leads to an ultra-ne grained microstructure
with elongated grains in the rolling direction (Fig. 4d) and by
increasing the number of cycles, the micrograph of ARB shows
both equiaxed and elongated grains (Fig. 4e). The fraction of the
ultrane grained regions increases with increasing the number of
cycles, i.e., strain. After 8 cycles of ARB (eq 6.4), the whole
volume of the material was lled with small and equiaxed
continuous recrystallized grains, as seen in Fig. 4f, and the average
grain size of these equiaxed recrystallized grains is below 100 nm.
This trend has been reported by many researchers in different
materials [1013].
A typical XRD pattern of TiNb microalloy steel is shown in
Fig. 5. The X-Ray diffraction patterns were recorded on the RD and
TD plane surfaces of the ARB processed sheet. Specimens for XRD
were prepared by polishing. XRD was carried out using an X-ray
diffractometer with Cu-K radiation. Fig. 5 shows the evolution of

A.A. Tohidi et al. / Materials Science & Engineering A 577 (2013) 4347

45

Fig. 3. Optical micrograph of longitudinal cross section of ARB samples subjected to (a) one, (b) three, (c) ve and (d) eight passes; the arrows shows some interfaces.

Fig. 4. SEM micrograph of (a) as-received, (b) three, (c) four, (d), (e) ve and (f) eight cycles of ARB.

Fig. 5. X-ray diffraction patterns for as-received condition and 8 pass ARB
condition.

texture caused by the ARB process. The relative height of the peaks
corresponding to the basal plane (110) increases signicantly after
the ARB process, which indicates that strong basal textures have
been created. Also the XRD pattern shows signicant peak broadening, indicative of ne grain size in the nonmetric range.

Fig. 6. Variation of Vickers hardness after various ARB cycles in TiNb

microalloy steel.

The development of hardness with the number of ARB cycles is

shown in Fig. 6 for TiNb microalloy steel. Hardness increased
rapidly by the rst few passes, so that after 34 ARB cycles, the
hardness increased by up to 2.2 times in comparison to the
as-received material. Thereafter, the hardness reaches a saturation
level and does not increase any further. The hardness of the

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A.A. Tohidi et al. / Materials Science & Engineering A 577 (2013) 4347

Fig. 7. Variation of hardness with thickness.

as-received TiNb microalloy steel was 134 HV. At the end of the
8th pass, the hardness has become 315 HV, indicating signicant
hardening. The rapid increase of hardness at the rst two passes
seems to be attributed to strain hardening [14]. The hardening
behavior showing saturation at large strains was commonly
reported in ultra-ne grain materials fabricated by the SPD process
[15]. As the grain size is reduced to nanoscale, the dislocation
mean free path and the number of dislocations that contribute to
work hardening are strongly reduced and the traditional concept
of pile-up at grain boundaries becomes very limited or it does not
occur at all. The dislocations are produced during deformation, but
they can also be stored or annihilated at the grain boundaries. The
grain boundaries can therefore act as sources as well as sinks for
dislocations. Thus, dynamic recovery becomes very common in
nanocrystalline/ultrane-grained materials and the competition
between dislocation generation during plastic deformation and
dislocation annihilation during recovery determines the steady
state dislocation density or grain size [16,17]. This is usually
reected in the mechanical properties of these materials, namely
at some point there is a saturation in hardness and strength.
Fig. 7 shows variation of hardness with thickness in TiNb
microalloy steel samples. The hardness of the specimens is a
constant value before the ARB. Each specimen after 1, 3, 5 and 8
cycles in the TiNb microalloy steel shows inhomogeneous distribution in the thickness direction, having higher values near the
surface and center. It is well known that the microstructural
evolution during the ARB process varies through the thickness of
the sheet due to the inhomogeneous shear distribution [13].
During the rst cycle, the surfaces in contact with the rolls and
at the interface of the two sheets are frictional forces. The
microstructural inhomogeneity and shear strain distribution are
especially dominant after the rst ARB cycle. This effect can be
clearly seen in Fig. 7 in terms of the hardness measured through
the thickness of the sheet. There is an overall increase in hardness
after the ARB cycle in comparison to the as-received state of TiNb
microalloy steel. However, the hardness after the rst cycle is
higher at the surface than in the middle of the sheet. After
subsequent rolling, the surfaces with the highest shear strain
migrate to the middle during the second cycle. This led to complex
distribution of plane strain and shear deformation, depending on
the location and the number of ARB cycles [18]. However, after a

sufcient number of ARB cycles the shear strain distribution as

well as the grain size becomes more homogeneous [13]. Similar
observations, were made in this work in terms of hardness, where
the hardness inhomogeneity seems to decrease with an increase in
number of ARB cycles.
The yield strength, the tensile strength and the elongation have
been determined in the tensile tests. The results are shown in
Fig. 8, plotted against the number of ARB cycles. Yield strength and
elongation in as-received state were 330 MPa and 34% respectively. The yield strength of the TiNb microalloy steel greatly
increases considerably to 668 MPa while the total elongation
drops down to 5.3% by one ARB cycle (equivalent strain 0.8). As
the number of ARB cycles further increases, the strength continuously increases and after 8 cycles of ARB reaches 1102 MPa,
which is 3 times higher than that of the as-received material. On
the other hand, the elongation of TiNb microalloy steel does not
change as much after the second ARB cycle and after 8 cycles the
elongation becomes 2.9%.
There are two major sources of limited ductility in nanocrystalline or UFG materials processed by ARB, namely low interlamellar
bond strength of the last bonded layer and low work hardening.
The absence of work hardening causes localized deformation and
leads to early tensile instability and thus low ductility [16]. Low
interlamellar bond strength of the last bonded layer additionally
contributes to premature failure, since it results in delamination of
the sheets.
The active strengthening mechanisms in Ti-Nb microalloy
steel include solid solution strengthening, precipitation strengthening, grain boundary strengthening and work hardening. In the
rst few cycles, the dominating strengthening mechanism in ARB
processed TiNb microalloy steel sample may be attributed to
strain hardening or dislocation strengthening [13]. Up to 3 cycles,
strain hardening or dislocation strengthening plays a main role in
the strength increase, and the formation of subgrain or dislocation
cells also contributes to the strength from 4 cycles. The increase in
strength was mostly due to the evolution of grain structure and
formation of UFG structure. 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 [13].
The difference between yield and tensile strength values is only
pronounced in the as received state, but diminishes upon further
ARB rolling. This clearly indicates that the strain hardening
potential of TiNb microalloy steel decreases with increasing
number of ARB cycles. In this material, limited strain hardening
can be attributed to a small grain size. By switching to the
nanoscale, the classical deformation behavior of crystalline materials may be changed as other deformation processes, like grain
boundary sliding, dislocation annihilation or twinning, become
dominating. The ARB structure has a high dislocation density

Fig. 8. Variation of mechanical properties in TiNb microalloy steel by number of

ARB cycles.

A.A. Tohidi et al. / Materials Science & Engineering A 577 (2013) 4347

which affects the deformation behavior as moving dislocations are

normally not stored in the grain interior, but rather at the grain
boundaries. Consequently dynamic recovery takes place mainly
along the grain boundaries. Hence the strain hardening capability
is reduced as dislocation annihilation and recovery can easily take
place at the grain boundaries [17,19].

4. Conclusion
TiNb microalloy steel with an ultra-ne structure was
obtained by accumulative roll bonding. The UFG material shows
higher hardness, yield and tensile strength compared to its
conventionally grained counterpart, but unfortunately shows only
limited ductility. Hardness and yield strength of UFG material are
typically 2.35 and 3.34 (respectively) times higher than that of the
conventionally grained counterpart. The elongation to failure
decreases after the rst few ARB cycles and is signicantly lower
in comparison to the as-received materials. In the UFG TiNb
microalloy steel the maximum elongation to failure in the rolling
direction reaches up to 2.9%.

47

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