Materials Science and Engineering A 527 (2010) 4043–4049

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Materials Science and Engineering A

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

Constrained groove pressing of low carbon steel: Nano-structure and

mechanical properties
F. Khodabakhshi, M. Kazeminezhad ∗ , A.H. Kokabi
Department of Materials Science and Engineering, Sharif University of Technology, Azadi Ave., Tehran, Iran

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

Article history: In this study a severe plastic deformation method called constrained groove pressing (CGP) is used for
Received 19 December 2009 imposing a high magnitude of strain into the low carbon steel sheets. Microstructural changes during
Received in revised form 28 February 2010 process are examined by X-ray diffraction and optical observations. The grain size evolution during severe
Accepted 1 March 2010
plastic deformation is studied using Williamson–Hall analysis on XRD pattern of the deformed samples.
In effective strain of 4.64, ferrite grains with a submicron size of 200–300 nm are achieved. The results
show that constrained groove pressing can effectively refine the coarse-grained structure to an ultra fine
Keywords:
grain range. Mechanical properties changes due to microstructure evolution are measured by tensile and
CGP
Low carbon steel
hardness tests. The results show that the constrained groove pressing process leads to decrease of work
X-ray diffraction hardening rate and increase of strain rate sensitivity of the sheets material. Finally, in cumulative strain
Mechanical properties of 4.64, a deformed sheet with grain size of 230 nm and ultimate tensile strength of 400 MPa is obtained.
Nano-structure © 2010 Elsevier B.V. All rights reserved.

1. Introduction
Bulk nano-structured materials have been mostly attracted in
materials science due to their unique physical and mechanical
properties [1]. Ultra fine grained (UFG) materials can be synthesized
by either bottom-up or top-down approaches. In the bottom-up
approach, the nano-structure is produced through atom-by-atom
and layer-by-layer arrangements that often leads to porous struc-
ture and is not applicable to industrial manufacturing [2]. In the
top-down approach, the bulk material’s microstructure is changed
to nano-structure utilizing severe plastic deformation (SPD) [3].
Refining the grain size of useful metals such as low carbon steel
is of great interest as the yield stress is increased with grain refine-
ment, significantly. This leads to an improvement in the strength to
weight ratio, which is a desirable property for automobile industry.
Severe plastic deformation (SPD) is one of the most efficient meth-
ods to produce ultra fine grained or nano-structured materials.
The principle of SPD processes includes increasing the dislocation
density by heavily uniform deformation, forming of dense disloca-
tion walls and acquiring ultra fine or nano-scale microstructure [4].
Materials produced by SPD are of great importance because of (1)
non-porous structure, (2) great mechanical properties such as high
strength and toughness and (3) proper dimension for mechanical
and physical testing [5].
∗ Corresponding author. Tel.: +98 21 66165227; fax: +98 21 66005717.
E-mail address: mkazemi@sharif.edu (M. Kazeminezhad).
The SPD processes decrease the grain size of materials into nano-
scale, thus transmission electron microscopy (TEM) and X-ray
diffraction (XRD) are two basic methods for grain size evaluation
of nano-structured material [6]. Transmission electron microscopy
can provide a direct image of the grain size distribution. How-
ever, grain overlapping leads to uncertainty and the reliability of
images depends on whether the limit area is a representative of the
original microstructure of the entire sample [6,7]. In contrast, the
indirect methods based on XRD line broadening have the advan-
tages of average over a much larger area of the sample and ease
of sample preparation [6]. X-ray line profile analysis has been well
used in studying the grain size, density and arrangement of dislo-
cations in deformed metals [8]. During the last decades, several
methods have been introduced for imposing the severe plastic
deformation to the metals [9–18]. Some of these methods are:
equal channel angular pressing (ECAP) [18], high pressure torsion
(HPT) [10], accumulative roll bonding (ARB) [17], repetitive cor-
rugation and straightening (RCS) [11], constrained groove rolling
(CGR) [14], constrained groove pressing (CGP) [16], etc. Within
these methods, only the four last methods are applicable for pro-
ducing nano-structured sheets.
Two major SPD processes of sheet are accumulative roll bond-
ing (ARB) and constrained groove pressing (CGP). The process of
ARB has been invented by Saito et al. [15,19], involves repetitive
bonding between two rolled plates and if perfect bonding is not
accomplished, the bonding interface may reduce the mechanical
properties of the products. Thus, ARB is less considered feasible
for severe plastic deformation of sheet metals. Constrained groove
pressing, originally proposed by Shin et al. [16], has the advantage

0921-5093/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2010.03.005
4044 F. Khodabakhshi et al. / Materials Science and Engineering A 527 (2010) 4043–4049

Fig. 1. Schematic of sections for optical microscopy observations, grooving (I, III) and flattening dies (II, IV).

of imposing more uniform severe plastic deformation on sheet met- Table 1

Chemical composition of the studied steel (wt.%).
als and has not bonding problem. The principle of CGP is subjecting
a material to a large amount of plastic shear deformation with Fe Base Al 0.0605 As <0.00030
asymmetrically grooved and flat dies pressing, alternatively [4] (see C 0.0527 Co 0.0048 Zr 0.0014
Si 0.0229 Cu 0.0128 Ca 0.00008
Fig. 1). Since this method has been recently invented, there are not
Mn 0.203 Nb 0.00048 Sb <0.00050
many works on it and it seems that more works should be carried P 0.006 Ti 0.00099 Ta 0.0014
out to investigate the evolution of material characteristics during S 0.0031 V 0.0033 B 0.00028
the process. Recently, some researches have been carried out on Cr 0.0088 W 0.0032 Zn 0.00031
mechanical properties and microstructure of aluminum and copper Ni 0.0281 Pb 0.0012
Mo 0.0024 Sn 0.0024
sheets, processed by CGP indicating that this process can have great
influence on mechanical properties of sheet metals such as increase
of yield strength and mean hardness [4,16,20–25]. Also, this pro- In the first stage flat sheet becomes corrugated which results in
cess has the ability of producing sub micrometer polygonized grain a 0.58 effective strain in deformed regions (Fig. 1(I)). Then in the
structure with well-defined grain boundary as that reported in the second stage, flat dies flatten the corrugated sheet by imposing an
work of Shin et al [16]. However, most of the previous works on extra 0.58 strain in reverse direction to the previously deformed
SPD of low carbon steel were on the equal channel angular pressing, sections (Fig. 1(II)). It is worth to note that in this stage the sheet
which produce bulk nano-structured materials [26–31] and many has two different regions, unstrained one with zero strain and shear
works were carried out on the SPD of IF steel sheets using ARB pro- strained one with 1.15 strain. After straightening, the specimen
cess [17,32–35]. Since the SPD of low carbon steel is important and is rotated 180◦ around the axis perpendicular to the plane of the
ARB has some disadvantages, in this study for the first time, CGP sheet and then the first stage is repeated (Fig. 1(III)). Then in fourth
method is carried out on the sheets of low carbon steel. Therefore stage, the corrugated sheet is flattened (Fig. 1(IV)). At the end of
the potential of CGP method in grain refinement and mechanical one CGP pass that contains four stages, a uniform effective strain
properties improvement of low carbon steel should be investigated. of 1.16 has been imposed throughout the specimen [5,16,22]. In
In this research, cumulative strain of 0–4.64 (each CGP pass the present study, as-received low carbon steel sheets with dimen-
imposes strain magnitude of 1.15 [16,22]) are imposed to the sion of 84 mm × 45 mm × 3 mm were used to study the effects of
low carbon steel sheets containing 0.06 wt% C to produce a high CGP process on grain refining and strengthening. The initial grain
strength nano-structured sheet and in following, by using optical size of material is 30 ␮m and its chemical composition is shown in
microscopy, tensile test, hardness tests and XRD, characteristics of Table 1. Fig. 2 shows the experimentally processed sample sheet
deformed sheets are investigated. that represents the shape of specimen after the first pressing stage.
XRD is employed to determine the grain size and to monitor In this study, Teflon layers that introduced in previous work [36]
the microstructural changes during SPD processes. Microstructures were used before each pass as a lubricant between low carbon steel
of CGPed sheets are analyzed through optical observations. Also,
the effect of imposing strain in the range of 0–4.64 into the sheets
on the strengthening behavior of them is investigated using some
mechanical tests such as tensile and hardness tests.

2. Experimental material and procedure

Schematic of CGP dies and one pass of CGP that includes four
pressing stages are shown in Fig. 1(I)–(IV). The pressings are per-
formed such that the gap between the upper die and the lower die is
the same as the sample thickness, resulting in pure shear deforma-
tion under plane strain condition at inclined regions of the sample. Fig. 2. Low carbon steel sheet after the first stage of CGP (εeff = 0.58).
 F. Khodabakhshi et al. / Materials Science and Engineering A 527 (2010) 4043–4049 4045

Fig. 3. The sections for hardness measurement.

sheet and dies. Using these layers can reduce the friction between
the sheet and dies, and this modification reduces the probability
of surface cracking and makes it possible to impose the cumula-
tive strain of 4.64 to the sheets through four passes. The pressing
force of process was supplied by using a 1000 kN hydraulic press-
ing machine at a ram speed of 0.05 mm s−1 . The loads applied for
pressing stages were in the range 50–65 kN.
To investigate the mechanical behavior of low carbon steel
sheets after CGP, tensile and hardness tests were carried out. After
CGP, tensile samples were cut from the deformed sheets that their Fig. 4. XRD pattern of as-received and CGPed low carbon steel sheets.
gage length aligned along the longitudinal direction of the pressed
sheet and machined with gage length of 32 mm according the ASTM
the lattice strain,  is the Bragg angle and f is a defined function in
E8M standard. All tensile tests were conducted at room tempera-
Refs. [6–8,37].
ture using an Instron tensile testing machine operating at a constant
In this method, B cos  is plotted against sin  and using a linear
rate of cross-head displacement and with an initial strain rate of
extrapolation to this plot, the intercept gives the cell size. How-
5 × 10−3 s−1 . Vickers hardness measurements were carried out on
ever, it should be considered that the environment in a commercial
the longitudinal A and B sections of deformed sheets (see Fig. 3) that
diffractometer is not ideal and instrumental broadening must be
A and B sections are the sheet surface and center of its thickness,
extracted in advance. In principle, the experimental profile is the
respectively. As shown in Fig. 3, hardness measurements is car-
convolution of the instrumental profile and the intrinsic profile
ried out along line a–a in A-section and along line b–b in B-section.
(pure diffraction profile). The intrinsic profile can be obtained by
The mean hardness values for two sections were achieved from 12
unfolding the experimental profile. The simplified method is based
measurements on each specimen.
on assumptions that the intrinsic and instrumental profiles can
The microstructures of deformed sheets were investigated after
be approximated by a bell-shaped function, such as the Cauchy
CGP using both optical microscopy and X-ray diffraction. In order
(Lorentz) or Gaussian function [6]. According to the assumption of
to examine the microstructure, the samples for optical microscopy
Cauchy or Gaussian shape, the integral breadths can be described
were prepared from both as-received and deformed specimens. The
using the Gaussian–Gaussian (GG):
samples of as-received specimen were selected from its surface
and longitudinal thickness planes in order to show microstructural 2
Bexp ∼
= B2 + Bins
2
(2)
differences in the planes. In Fig. 1, a schematic illustration of the
samples in thickness planes (B-section) of deformed specimen is where Bexp , B, and Bins are the integral breadth of experimental pro-
shown. For optical microscopy, samples were ground on papers, file, intrinsic profile, and instrumental profile, respectively. There
polished and then etched in a solution of CH3 OH containing 3% are different reliable model-based approaches of XRDLPA (X-ray
HNO3 . Diffraction Line Profile Analysis), but in this study Williamson-Hall
To investigate the microstructure evolution of sheets during approach was used due to its simplicity and good reliable results.
process, XRD measurements were carried out on a Philips X-ray Typical XRD pattern of low carbon steel is shown in Fig. 4. As
diffractometer equipped with a graphite monochromator using Cu can be seen, the diffraction from three crystalline planes is more
K␣ radiation between 35◦ to 110◦ 2-theta range and the results intense than that of others; (1 1 0), (2 0 0) and (2 1 1). Therefore, in
were analyzed using Williamson–Hall method. Full-width at half- this study the diffractions of these three peaks on all samples are
maximum (FWHM) for all peaks was measured using the software considered to find the evolution of grain size.
configured with the XRD system. The X-ray patterns of samples
were achieved at a step width of 0.02◦ . For calibration of the instru- 3. Results and discussion
mental line broadening, a fully mixture of coarse TiC and B4 C
powders was tested in the same condition. 3.1. Mechanical properties
XRD profiles can be evaluated as follows:
Two principal crystal imperfections in nano crystalline mate- Figs. 5 and 6 show the tensile behavior of as-received and two
rials, i.e., small crystallite size and lattice distortion, cause peak pass deformed samples, respectively. From the figures, it can be
broadening compared with the Bragg peak that results from per- observed that the deformation through CGP leads to decrease of
fect crystal diffraction [6,7]. Grain size and lattice microstrain can be uniform elongation of samples from 0.259 to 0.022. It means that
accordingly determined by measuring the deviation of line profile plastic instability starts earlier in the CGPed material and necking
from perfect crystal diffraction. For example, the Williamson–Hall occurs in preliminary stages of tensile deformation. The early onset
equation can calculate strain and crystalline size of materials as of necking in the CGPed material is due to the low-hardening rate
follows [37]: (low n in Hollomon’s relation [38]). However, it can be seen that
the fraction of non-uniform elongation to all, is markedly increased
K
B cos  = + f (ε) sin  (1) from 0.266 to 0.667 after CGP process. This means that for CGPed
t sheet the major of tensile strains are obtained in the state of plastic
where B is the integral breadth of the XRD profile, K is the Scherer instability and the material has high strain rate sensitivity (high m
constant, t is the crystallite size,  is the wavelength of X-ray, ε is in Hollomon’s relation [38]). These evidences indicate that plastic
4046 F. Khodabakhshi et al. / Materials Science and Engineering A 527 (2010) 4043–4049
Fig. 5. Tensile stress–strain curve of as-received low carbon steel.
Fig. 6. Tensile stress–strain curve of low carbon steel after two passes of CGP.
deformation through CGP increases the superplasticity tendency
of low carbon steel sheets that is acceptable considering the grain
refinement during CGP process. Similar result has been reported
for CGPed aluminum sheets [36].
The tensile properties variations (yield stress, ultimate tensile
strength and elongation) of the deformed sheets versus magni-
tude of imposed strain are shown in Fig. 7, this measurement is
carried out for as-received, one, two, three and four CGP pass spec-
imens. The general trend that can be found from Fig. 7 is that both
yield stress and UTS of samples are increased during deformation
until second pass of CGP, however for the two last passes, strength
drop is observed. The elongation is decreased with increasing the
strain.
The as-received sheet had an ultimate tensile strength of
288 MPa. After two pass of CGP ultimate tensile strength is
Fig. 7. Variations of mechanical properties of low carbon steel sheets during CGP
process.
Fig. 8. The Vickers hardness profile along the length of the specimen in A-section.
Fig. 9. The Vickers hardness profile along the length of the specimen in B-section.
increased from 288 to 447 MPa. The yield strength of the as-
received sheet was 204 MPa and after first pass, the yield strength
is increased to 412 MPa. Increasing the strength of material dur-
ing SPD is common and arises from the work hardening and grain
refining mechanisms. Previous papers on CGP of copper and alu-
minum explained the dropping phenomenon using two theories;
microcracking and flow softening [5,36]. The achieved strength val-
ues show a similar trend reported for aluminum and copper by
researchers in previous works [4,16,21,22,25,36].
3.2. Hardness
The hardness distributions across the length of the specimens
in sections A and B are shown in Figs. 8 and 9, respectively. In
both sections, the hardness is increased with increasing the pass
number. The uniformity of hardness is discussed later using the
Fig. 10. The mean hardness value of the sheets versus pass number in A-section.
 F. Khodabakhshi et al. / Materials Science and Engineering A 527 (2010) 4043–4049 4047

Fig. 11. The mean hardness value of the sheets versus pass number in B-section.

data presented in these figures. The mean values of hardness Fig. 12. The variation of I.F. with CGP pass number for A and B sections.
as a function of pass number in sections A and B are shown in
Figs. 10 and 11, respectively. As can be seen the hardness values
changes during the third and fourth passes that it will be discussed
of sheets are increased rapidly through first pass. However in
later.
the following passes, the rate of hardness increasing is reduced.
In order to investigate the uniformity of hardness distributions,
As interesting point that can be concluded from the results in
the inhomogeneity factor (I.F.) is used. This can be calculated by [5]:
Figs. 10 and 11 is different initial hardness values in sections A 
and B of as-received specimen and the same hardness values n 2
i=1
(Hi − H̄) /n − 1
achieved in both sections of four pass CGPed specimen. This can be I.F. = × 100 (3)
attributed to the less effect of strain magnitude on microstructure H̄

Fig. 13. Optical microstructures in two sections: (a) in the as-received condition from the specimen surface, (b) in the as-received condition from the specimen thickness,
(c) after the first pressing from A-1 region, (d) after the second pressing from A-2 region, (e) after the third pressing from B-1 region, (f) after the fourth pressing from B-2
region.
4048 F. Khodabakhshi et al. / Materials Science and Engineering A 527 (2010) 4043–4049
where n is the number of hardness measurements on each spec-
imen, Hi is the hardness value of i-th measurement, and H̄ is the
mean hardness value. In general, less I.F. value indicates higher
homogeneity of mechanical properties. Fig. 12 shows the I.F. of
specimens in two sections. As can bee seen, I.F. of hardness val-
ues in B-section is lower than that in A-section. This can be related
to the pure shear deformation occurs in B-section and existence of
additional one due to friction effect in A-section, i.e. interface of
sheet and dies. Also, it can be observed that for two sections, the I.F.
of one pass CGPed specimen is increased compared with that of as-
received one. For CGPed sheets, the I.F. is decreased with increasing
the pass number indicating increase of strain homogeneity.
3.3. Microstructure evolution
The optical microstructures of the CGPed steel sheets as a func-
tion of pass number, observed on the surface and thickness planes
of the sheets in longitudinal direction, are shown in Fig. 13. Opti-
cal observations in the thickness plane is carried out from the
center of sheet thickness that also shown in coordinate systems
in Fig. 13. The as-received steel consists of approximately 6 vol%
pearlite (dark contrast) and the remainder is ferrite (bright con-
trast). In as-received condition, the microstructures from the sheet
surface and sheet thickness are shown in Figs. 13(a) and (b), respec-
tively. It is clearly shown in Fig. 13(c) that the initial equiaxed grains
of the as-received sample, with size of 30 ␮m, are elongated along
the direction of 45◦ inclined to the longitudinal axis (A-1 region
in Fig. 1(I)) by the first press. As shown in Fig. 13(d), the sec-
ond press results in smaller and more irregular equiaxed grains
with dim grain boundary contours (A-2 region in Fig. 1(II)), com-
pared with that in the as-received microstructure. In Figs. 13(e)
and (f), similar trends are observed in third and fourth pressings
from B-1 (Fig. 1(III)) and B-2 regions (Fig. 1(IV)), respectively. Fur-
ther presses show similar morphological changes: with an odd
number of presses, the grains are severely elongated along the
direction of 45◦ inclined to the longitudinal axis and the grains are
restored to their equiaxed shape with the subsequent even number
of presses.
By analyzing the XRD patterns, evolution of low carbon steel
cell size during CGP process is calculated and shown in Fig. 14. As
can bee seen during first pass of CGP, the coarse-grained low carbon
steel (with average initial grain size of 30 ␮m) refines to a structure
with cell size of 346 nm. However, after this rapid refinement, the
rate of refining is decreased and after fourth pass of CGP, the cell
size is about 231 nm.
Dislocation theories can interpret this trend; a relationship
between imposed strain rate and rate of dislocation generation is
obtained if the Orowan equation is considered on a larger time scale
Fig. 14. The cell size versus CGP pass number and imposed strain.
[39]:
•
•+ 
 = (4)
bL
•+
where  is the rate of dislocation density increasing; L is the dislo-
•
cation free path; b is the Burgers vector and  is the resolved strain
rate. Since the cell size (d) is proportional to −1/2 [4,40], by consid-
ering Eq. (4), it seems that deformation can refine the structure in a
uniform manner. However, the second type of dislocation reactions
during deformation that is called dynamic recovery prohibits this
steady rate grain refinement. The main role of dynamic recovery
is dislocation annihilation and since the rate of dynamic recovery
is proportional to the material dislocation density, rate of dynamic
recovery is increased through straining and causes to decrease the
rate of grain refinement at large strains. Therefore, it is acceptable
to observe intensive grain refinement at the initial passes of CGP
and the reduced rate of refinement at the following passes. Com-
paring the TEM observations reported by Fukada et al. [26] in the
ECAE of the same composition steel with the achieved results of
XRD analysis shows that both processes have similar effect on grain
size evolution of low carbon steel.
4. Conclusions
In the present study low carbon steel sheets were subjected to a
severe plastic deformation (SPD) method called constrained groove
pressing (CGP) and a cumulative strain of 4.64 was imposed to the
sheets. Also, the effect of CGP on grain size and mechanical proper-
ties evolutions of the sheets were investigated. The main findings
of this study can be presented as follows:
1. Yield stress and UTS of sheets are increased during straining until
two pass to 400 and 450 MPa, respectively, and further deforma-
tion than that causes to strength drop.
2. The CGP process causes to decrease of work hardening rate
and increase of strain rate sensitivity compared with that of
as-received specimen.
3. Initial hardness values in sections A and B of as-received speci-
men is different and the same hardness achieved in both sections
of four pass CGPed specimen.
4. The I.F. of hardness values in B-section is lower than that in A-
section. The I.F. of one pass CGPed specimen for both sections
is increased compared with that of as-received one. For CGPed
sheets, the I.F. is decreased with increasing the pass number
indicating increase of strain homogeneity.
5. Grain size of low carbon steel sheets is decreased by increasing
the pass number of CGP process. The maximum rate of grain
refinement is during initial pass and with increasing the CGP
pass number the rate is decreased.
6. A submicron ferrite grain size of 200–300 nm was achieved in
low carbon steel sheets by imposing a severe plastic strain of
4.64 utilizing the constrained groove pressing technique.
Acknowledgements
The authors wish to thank the research board of Sharif Univer-
sity of Technology for the financial support and the provision of the
research facilities used in this work.
References
[1] R.Z. Valiev, R.K. Islamgaliev, I.V. Alexandrov, Prog. Mater. Sci. 45 (2000)
103–189.
[2] P.G. Sanders, J.A. Eastman, J.R. Weertman, Acta Mater. 46 (1998) 4195–4202.
[3] Y.W. Tham, M.W. Fu, H.H. Hng, M.S. Yong, K.B. Lim, J. Mater. Process. Technol.
192/193 (2007) 575–581.
 F. Khodabakhshi et al. / Materials Science and Engineering A 527 (2010) 4043–4049 4049

[4] E. Hosseini, M. Kazeminezhad, A. Mani, E. Rafizadeh, Comput. Mater. Sci. 45 [22] A. Krishnaiah, U. Chakkingal, P. Venugopal, Scripta Mater. 52 (2005) 1229–1233.
(2009) 855–859. [23] K. Peng, L. Su, L.L. Shaw, K.W. Qian, Scripta Mater. 56 (2007) 987–990.
[5] E. Rafizadeh, A. Mani, M. Kazeminezhad, Mater. Sci. Eng., A 515 (2009) 162–168. [24] K. Peng, Y. Zhang, L.L. Shaw, K.W. Qian, Acta Mater. 57 (2009) 5543–5553.
[6] Z. Zhang, F. Zhou, E.J. Lavernia, Metall. Mater. Trans. A 34A (2003) 1349–1355. [25] J. Zrnik, T. Kovarik, Z. Novy, M. Cieslar, Mater. Sci. Eng., A 503 (2009) 126–129.
[7] P. Mukherjee, A. Sarkar, P. Barat, S.K. Bandyopadhyay, P. Sen, S.K. Chat- [26] Y. Fukuda, K. Oh-ishi, Z. Horita, T.G. Langdon, Acta Mater. 50 (2002) 1359–1368.
topadhyay, P. Chatterjee, S.K. Chatterjee, M.K. Mitra, Acta Mater. 52 (2004) [27] D.H. Shin, B.C. Kim, Y.-S. Kim, K.-T. Park, Acta Mater. 48 (2000) 2247–2255.
5687–5696. [28] D.H. Shin, I. Kim, J. Kim, K.-T. Park, Acta Mater. 49 (2001) 1285–1292.
[8] E. Schafler, M. Zehetbauer, T. Ungàr, Mater. Sci. Eng., A 319–321 (2001) 220–223. [29] D.H. Shin, J.-J. Pak, Y.K. Kim, K.-T. Park, Y.-S. Kim, Mater. Sci. Eng., A 325 (2002)
[9] I.V. Alexandrov, R.Z. Valiev, Nanostruct. Mater. 12 (1999) 709–712. 31–37.
[10] Z. Horita, T.G. Langdon, Scripta Mater. 58 (2008) 1029–1032. [30] D.H. Shin, J.-J. Pak, Y.K. Kim, K.-T. Park, Y.-S. Kim, Mater. Sci. Eng., A 323 (2002)
[11] J. Huang, Y.T. Zhu, D.J. Alexander, X. Liao, T.C. Lowe, R.J. Asaro, Mater. Sci. Eng., 409–415.
A 371 (2004) 35–39. [31] D.H. Shin, K.-T. Park, Mater. Sci. Eng., A 410/411 (2005) 299–302.
[12] J.Y. Huang, Y.T. Zhu, H. Jiang, T.C. Lowe, Acta Mater. 49 (2001) 1497–1505. [32] A.L.M. Costa, A.C.C. Reis, L. Kestens, M.S. Andrade, Mater. Sci. Eng., A 406 (2005)
[13] J. Kratochvíl, M. Kruzík, R. Sedlácek, Acta Mater. 57 (2009) 739–748. 279–285.
[14] J.W. Lee, J.J. Park, J. Mater. Process. Technol. 130/131 (2002) 208–213. [33] N. Kamikawa, T. Sakai, N. Tsuji, Acta Mater. 55 (2007) 5873–5888.
[15] Y. Saito, N. Tsuji, H. Utsunomiya, T. Sakai, R.G. Hong, Scripta Mater. 39 (1998) [34] N. Kamikawa, N. Tsuji, Y. Minamino, Sci. Technol. Adv. Mater. 5 (2003) 163–172.
1221–1227. [35] N. Tsuji, R. Ueji, Y. Minamino, Scripta Mater. 47 (2002) 69–76.
[16] D.H. Shin, J.-J. Park, Y.-S. Kim, K.-T. Park, Mater. Sci. Eng., A 328 (2002) 98–103. [36] E. Hosseini, M. Kazeminezhad, Mater. Sci. Eng., A 526 (2009) 219–224.
[17] N. Tsuji, Y. Saito, H. Utsunomiya, S. Tanigawa, Scripta Mater. 40 (1999) 795–800. [37] P. Mukherjee, A. Sarkar, P. Barat, Mater. Charact. 55 (2005) 412–417.
[18] R.Z. Valiev, T.G. Langdon, Prog. Mater. Sci. 51 (2006) 881–981. [38] G. Dieter, Mechanical Metallurgy, McGraw-Hill book Company, New York,
[19] Y. Saito, H. Utsunomiya, N. Tsuji, T. Sakai, Acta Mater. 47 (1999) 579–583. 1986.
[20] M. Kazeminezhad, E. Hosseini, Mater. Des. 31 (2010) 94–103. [39] F. Roters, D. Raabe, G. Gottstein, Acta Mater. 48 (2000) 4181–4189.
[21] A. Krishnaiah, U. Chakkingal, P. Venugopal, Mater. Sci. Eng., A 410/411 (2005) [40] Y. Estrin, A. Molotnikov, C.H.J. Davies, R. Lapovok, J. Mech. Phys. Solids 56 (2008)
337–340. 1186–1202.