Journal of Manufacturing Processes 14 (2012) 20–25

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Journal of Manufacturing Processes

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

Technical paper

Work hardening and mechanical properties of severely deformed AA3003 by

constrained groove pressing
F. Khakbaz, M. Kazeminezhad ∗
Department of Materials Science and Engineering, Sharif University of Technology, Azadi Avenue, Tehran, Iran

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

Article history: A severe plastic straining method, called constrained groove pressing, is used to improve the microstruc-
Received 4 April 2011 ture and mechanical properties of non-hardenable 3003 Al–Mn alloy. Williamson–Hall method is utilized
Received in revised form 18 July 2011 to measure the grain size from X-ray diffraction patterns of deformed samples. The results show that ultra-
Accepted 20 July 2011
fine grained 3003 alloy having grain size of 580 nm can be successfully produced by constrained groove
Available online 6 August 2011
pressing at room temperature. Mechanical properties of sheets, examined by tensile test, are approx-
imately exhibited 170% improvement in comparison with those of annealed sample. Also, comparing
Keywords:
the achieved results with those of aluminum 1100 alloy confirms the rapid rate of grain refinement and
AA3003
Constrained groove pressing
mechanical properties improvement in 3003 alloy. This is attributed to the presence of fine dispersoids
Work hardening of Al6 Mn in microstructure of the alloy. Tensile tests demonstrate that the work hardening rate of con-
Grain size strained groove pressed sheet is increased in comparison with that of annealed samples. Investigating of
the work hardening by a model reveals why improvement stops after third pass and also work hardening
rate diagrams show that only one stage of work hardening is detectable for the sheet after three passes of
constrained groove pressing, while in lower pass numbers, more work hardening stages can be observed.

© 2011 The Society of Manufacturing Engineers. Published by Elsevier Ltd. All rights reserved.

1. Introduction
One of the methods for improving the mechanical properties
of metals is production of ultra-fine grains (nanocrystalline or sub
micron). The interest in producing metals with very small grains
is due to the fact that a reduction in grain size leads to increase
the strength and toughness of the material at ambient tempera-
ture, and there is also a potential for achieving good formability and
superplastic ductilities [1]. Traditionally, small grains are produced
by the development of appropriate thermomechanical processing
routes. However, this procedure may be different for each alloy and
the smallest grain size achieved through this method is often in the
range of 1–10 ␮m. As a consequence of these limitations, a sim-
ple method for fabricating bulk nanostructured metals is required.
Severe plastic deformation (SPD) is well-developed process for
grain refinement, and several techniques have been invented, such
as, Equal Channel Angular Pressing (ECAP) [2,3], High Pressure
Torsion (HPT) [4], Accumulative Roll Bonding (ARB) [5] and Con-
strained Groove Pressing (CGP) [6]. The last two methods can
produce nanostructured sheets. ARB process involves repetitive
∗ Corresponding author. Tel.: +98 21 66165227; fax: +98 21 66005717.
E-mail address: mkazemi@sharif.edu (M. Kazeminezhad).
bonding between two rolled plates, but, if perfect bonding is not
accomplished, the bonding interfaces may reduce the mechanical
properties of ARBed material. Thus, ARB is less considered feasi-
ble for severe plastic deformation of sheet metals [7]. In 2002, Shin
et al. [6] described the CGP method based on the corrugating and
straightening of sheets, which imposes the uniform shear deforma-
tion to the sheets. The CGP process has been successfully applied
to aluminum 1100 alloy [8,9], copper [10], Cu–Zn alloy [11] and
low carbon steel [7]. The researchers indicate that CGPed mate-
rials have a structure with submicron size and exhibit very good
mechanical properties. In this study, CGP process is carried out on
the sheet of aluminum alloy 3003 at room temperature. In 3003
aluminum alloy, Mn increases work hardening rate because of pro-
ducing fine particles of Al6 Mn and solid solution condition. These
particles can increase the rate of dislocation generation as a result
of Frank sources [12]. The main weakness of this class of aluminum
alloys is non-hardenable for strengthening. So, with the aid of work
hardening in SPD processes, the strength can be upgraded to higher
values.
In this research, the strains of 0–4.64 are imposed to 3003 sheets
and then by using tensile test, hardness test and XRD, the mechan-
ical properties and microstructure evolutions of deformed sheets
are investigated. The aim is to clarify whether it is possible to pro-
duce 3003 alloy sheet with ultra-fine grains and high strength by
using CGP technique.

1526-6125/$ – see front matter © 2011 The Society of Manufacturing Engineers. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.jmapro.2011.07.001
 F. Khakbaz, M. Kazeminezhad / Journal of Manufacturing Processes 14 (2012) 20–25 21

2. Experimental procedure Table 1

Chemical composition of the studied Al–Mn alloy (wt.%).

2.1. Constrained groove pressing Element wt%

Al Base
The CGP dies and one pass of the process which contains four Mn 0.944
stages are exhibited in Fig. 1. Also, the practical images of two stages Fe 0.353
can be seen in this figure. In the first step of groove pressing, a spec- Si 0.222
imen is placed in the die with slight gap which is equal to the sheet Cu 0.065

thickness. In each grooving stage, the inclined region of sample is

subjected to pure shear, under plane strain condition [6].
In the first pressing, the equivalent strain of 0.58 is imposed to
the work piece. Then in the second stage, by flat pressing, the previ-
ous deformed region is subjected to another 0.58 strain in reverse
direction. So after first flattening press, the cumulative strain of
1.16 is applied to the deformed regions of sheet. After the second
stage, the specimen is rotated 180◦ around the pressing direction.
By repeating the groove pressing stage, strain of 0.58 is imposed to
the previous undeformed region. At the end, the specimen is flat-
tened again and one pass of CGP with total strain of 1.16 in whole
specimen is completed.
The repetition of this process leads to a large amount of plas-
tic strain in sample with no dimension change and ultra-fine
microstructure is achieved [13].
2.2. Material
In this study, aluminum alloy 3003 sheet with initial dimension
of 84 mm × 70 mm × 3 mm is processed with CGP technique. The
chemical composition of the alloy is shown in Table 1. Prior to CGP,
specimens were fully annealed at 450 ◦ C for 3 h.
2.3. Microstructural examinations
After CGP of Al–Mn sheets, for investigating the cell/grain size
and microstructure changes, X-ray diffraction analysis was used. To
measure grain size of CGPed sheets, X-ray analysis was carried out
on a Philips X-ray using Cu K␣ radiation, from 10◦ to 80◦ 2-theta
range. Samples for XRD were selected from the center of the sheets.
Grain size was calculated according to the peak broadening, with
Williamson–Hall method. In this method lattice strain and grain
size can be calculated using Eq. (1):
K
B cos  = + f (ε) sin  (1)
d
where B is the integrated breath of XRD profile, K is the Scherer
constant,  is the wave length of X-ray (1.54 Å for Cu K␣), d is the
grain size, ε is the lattice strain,  is the Brag angle and f(ε) is a

Fig. 1. CGP process stages, (a) first grooving stage, (b) first flattening stage, (c) second grooving stage, (d) second flattening stage, (e) practical image of grooving stage, (f)
practical image of flattening stage.
22 F. Khakbaz, M. Kazeminezhad / Journal of Manufacturing Processes 14 (2012) 20–25
Fig. 2. X-ray diffraction pattern of three passes CGPed 3003 alloy.
defined function in Refs. [14,15]. If B cos  is plotted versus sin ,
the intercept of linear extrapolation gives the grain size and the
slope of the line defines the value of lattice strain. Note that the
experimental profile is the convolution of instrumental profile and
the intrinsic profile (pure diffraction profile). The intrinsic profile
can be obtained by unfolding the experimental profile. For this pur-
pose one of the Cauchy–Cauchy (CC), Gaussian–Gaussian (GG), or
Cauchy–Gaussian (CG) relationships must be used. CG relationship
is given by:
 2
ˇ Bins
=1−
Bexp Bexp
where Bexp , ˇ and Bins are the integral breath of experimental pro-
file, intrinsic profile and instrumental profile, respectively [16]. An
X-ray diffraction pattern of three passes CGPed sheet is shown in
Fig. 2. In order to achieve more reliable results, integral breath is
measured by CG equation and also high intensity peaks are selected
for calculating grain size.
2.4. Mechanical examinations
To investigate the mechanical properties of CGPed Al–Mn
sheets, tensile and hardness tests were used. After process, work
pieces were cut and tensile samples were prepared according to
ASTM E8M standard. All tensile tests were carried out at room tem-
perature in order to impede the effects of dynamic recovery. Strain
rate was 10−4 s−1 and Vickers hardness values were measured in
longitudinal direction of the CGPed sheets.
It should be noted that all of data were achieved from three to
four measurements.
3. Results and discussion
There are several techniques for measuring cell/grain size after
severe plastic deformation. Using XRD for studying microstruc-
ture of bulk nano-materials is well-developed in prior researches
[14,16], and the reliability of this method has been proved from
TEM observations [9,17,18]. This technique has some advantages
in comparison with TEM, such as investigating over a much larger
area of samples and ease of sample preparation [7]. Fig. 3 shows the
variation of cell/grain size, calculated by Williamson–Hall method,
versus imposed strain to the sheets. The initial coarse-grained
Al–Mn (30–35 ␮m) is refined to microstructure with grain size
of 580 nm after three passes of constrained groove pressing. This
Fig. 3. The grain size versus imposed strain.
refinement is the major effect of severe straining. As can be seen
in Fig. 3, after a sudden drop in grain size through first and second
passes, rate of refinement is decreased by imposing third pass and
also grain size is approximately constant in fourth pass. The anni-
hilation of dislocations due to dynamic recovery through straining
reduces the rate of grain refinement. In other SPD processes of
Al–Mn alloy, such as ECAP [19] and ARB [20], this trend has been
confirmed. The grain size of 580 nm in third pass is smaller than
that reported by Xing et al. [20] after 8 passes of ARB process. The
larger grain size in latter research may be due to ARB process in
(2) 200 ◦ C carried out in order to achieve perfect bond. In this temper-
ature the dislocation mobility and thus the rate of dynamic recovery
are increased in comparison with that carried out in this study at
room temperature. Therefore, it is reasonable to achieve a smaller
grain size through CGP which can be carried out at room temper-
ature. Tensile behaviors of severely deformed and annealed sheets
are shown in Fig. 4. Uniform elongation is decreased from 0.39 for
annealed one to 0.05 for three passes CGPed one. As a consequence
of severe cold work on sheets, with increasing strain, plastic insta-
bility occurs in early stages of deformation. Khodabakhshi et al. [7]
and Hosseini et al. [9], in deformation behavior of low carbon steel
and pure aluminum after CGP, have reported that the major of ten-
sile strain is obtained in the state of plastic instability. Thus, the
tendency of superplasticity is enhanced which can be attributed
to the grain refinement occurs by severe plastic deformation. In
Fig. 4, general forms of stress-strain curves show fast drop after
UTS. This form is usual for materials having grain size between 400
and 1000 nm, which Yu et al. [21] reported in their work. Therefore,
this fact can confirm the validity of grain sizes measured by XRD
analysis in this study.
With increasing the strength of the alloy after constrained
groove pressing, the tensile elongation is decreased and this man-
ner can be justified by studying work-hardening behavior of the
deformed sheets. The work-hardening behavior has been mod-
eled by variety of expressions, but, for the present alloy, a suitable
theoretical framework for the work-hardening modeling has been
established by Kocks et al. [22]. This model is based on disloca-
tion density () which acts as an internal variable. The evolution
of dislocation density in the material is dependent on a balance
between dislocation storage and dislocation annihilation as a result
of dynamic recovery [23]. Dislocation storage occurs when the
mobile dislocations are immobilized by obstacles after traveling
the distance of L to provide a plastic strain of Mdε [22]:
Mdε = bLd (3)
 F. Khakbaz, M. Kazeminezhad / Journal of Manufacturing Processes 14 (2012) 20–25
Fig. 4. Tensile behavior of (a) annealed and (b) CGPed sheets.
where M is the Taylor factor (3 for fcc metals), ε is the strain and
b is Burgers vector (2.85 × 10−10 cm). Dynamic recovery occurs
as a result of dislocation cross slip, rearrangement, and annihila-
tion which can be considered to be proportional to the dislocation
density, so the total dislocation storage, d/dε, including dynamic
recovery, can be given by:
d
1  tion of dislocations due to dynamic recovery (third term in Eq.
=M − k2 
dε bL
Free path of L in the present alloy is affected by the presence of Mn in
the matrix as well as in the particles of Al6 (Mn,Fe). Several different
equations are defined for considering this effect (for example see
Ref. [24]), but, for simplicity of the equations, it can be considered
√
as L = ˇ/ . So, Eq. (4) can be written as:
d √ tion density (as can be seen in Fig. 6) after imposing the strain of
= M(k1  − k2 )
dε
where k1 and k2 are the constants. Another term that should be con-
sidered in Eq. (5) is the geometrically necessary dislocations (GND)
which are required to accommodate the deformation incompati-
bility at grain boundaries due to the orientation change across a
boundary [25]. Thus, G assumed for GND generation is dependent
on grain size, but, as it is not directly dependent on dislocation
density, it can be considered as the following equation:
dG
= MKG
dε
where KG is a constant.
23
Fig. 5.  plot versus normalized stress for CGPed aluminum 3003 sheets.
So, Eq. (5) becomes:
d √
= M(KG + k1  − k2 ) (7)
dε
√
Integration of Eq. (7) together with  = MaGb , gives [26]:
M 2 0 s M 3 (aGb)2 KG M 2 0

s
2
 = + − − (8)
4 2 s 2
where a is a constant, G is the shear modulus,  = d/dε;  0 = aGbk1 /2
and  s = MaGb(k1 /k2 ). In fact,  0 is the maximum value of work
hardening and  s is the value of stress where  = 0. According to this
equation, variation of  versus  shows the parabolic trend which
has the slop of  0 in coordinate origin and maximum of ( 0  S )/4 in
 = ( S )/4. By plotting,  (Fig. 5) versus normalized stress ( −  y ),
it is possible to calculate the constants in Eq. (7). Therefore, the
rate of dislocation generation in the alloy during cold work can be
written as:
d √
= M(9.4 × 1014 + 94  − 19.3 × 108 ) (9)
dε
By considering  = 1011 m−2 for annealed condition and explicit
solving of Eq. (9), it is possible to calculate the variation of dis-
location density versus imposed strain (Fig. 6). As it can be seen in
Fig. 6, after three passes of constrained groove pressing, dislocation
generation reaches a plateau which likely arises from annihila-
(4) (9)). Note that the variation of mechanical properties also shows
similar trend which means after applying three passes of deforma-
tion, the rate of improvement is decreased. For more clear vision
on deformation behavior of 3003 alloy, the results are compared
with mechanical properties of CGPed 1100 alloy and illustrated in
Fig. 7. By applying first pass a very sharp change in UTS and YS is
observed for both alloys. This is due to drastic change in disloca-
(5) 1.16. After pass one, the values for 3003 alloy are higher than those
for 1100 alloy. To understand this behavior, detailed microstruc-
tural investigation is needed, which is found from XRD patterns
shown in Fig. 2. Addition of Mn to Al, leads to the formation of
fine dispersoids of Al6 Mn (0.5 ␮m average diameter) [27]. Thus,
in dispersoid-containing alloy, it is expected that with increas-
ing strain the average misorientation of formed cells is increased
more rapidly than that of single phase alloy [12]. So, the rate of
strength improvement is increased and by fewer numbers of passes
a high strength can be obtained. Dispersoids also expedite the
(6)
effect of dynamic recovery and the rate of strength improvement is
decreased in lower strains. The aggregation of dislocations around
24 F. Khakbaz, M. Kazeminezhad / Journal of Manufacturing Processes 14 (2012) 20–25
Fig. 6. Variation of dislocations versus imposed straining.
particles leads to the formation of cells or new grain boundaries.
On the other hand, dynamic recovery can occur and annihilation
of dislocations in higher strains during CGP causes to reduce the
rate of strength improvement. In Fig. 7, strength drop after apply-
ing fourth pass can be observed, but in 1100 alloy this phenomenon
occurs in higher numbers of passes. Dropping in strength has been
reported in CGPed Cu [10], pure Al [9] and low carbon steel [7]. Two
main reasons for strength dropping phenomenon are explained in
these reports as: flow-softening and micro-cracks.
As can be seen in Fig. 7, elongation of 3003 alloy is higher than
that of 1100 alloy. To obtain better elongation, Tsuji et al. [28] pro-
posed that it is necessary to enhance work-hardening of the matrix
by dispersion of fine second phase particles. So, enhanced ductility
of 3003 alloy in comparison with that of 1100 alloy is attributed
to the presence of such particles in microstructure. Mean hardness
values of 1100 and 3003 also exhibit similar trend described for
strength (Fig. 8).
Grain size has an important role in enhancement of mechani-
cal properties. According the Hall–Petch equation, strength has a
relationship with D−1/2 , where D is grain size. The strength data
of CGPed samples show a good agreement with Hall–Petch equa-
tion. Fig. 9 represents this relation for 1100 and 3003 alloys. As it
can be seen, the slope of fitted line for 3003 alloy is higher than
that for 1100 alloy. It shows that in smaller strains, rate of work
hardening for 3003 is higher and three passes of CGP are enough
Fig. 7. Variations of mechanical properties of 3003 and 1100 [9] aluminum alloys
versus imposed strain.
Fig. 8. Mean hardness values of CGPed 1100 [9] and 3003 alloys.
to obtain good mechanical properties. With decreasing the rate of
improvement in mechanical properties during latest CGP passes
(as described), the rate of grain refinement is also decreased. So,
it is important to notice that the role of grain size on strength is
more than that of dislocation density. On the other hand, in low
strains both increasing in dislocation density and decreasing the
grains size, and, in high strains decreasing the grain size, have the
major effect on mechanical properties.
Another interesting behavior of the CGPed Al–Mn sheets is vari-
ation of work hardening rate with increasing of pass number shown
in Fig. 10. By observing the figure, different steps are detectable:
first is non-linear stage of II, then a short-range parabolic stage
of III and at last there is stage IV, which characterizes by small
change in work hardening rate in comparison with that in other
steps. In Fig. 10, difference in slopes of curves separates these stages
(dash lined). The fact claimed from this figure, which known as
Kocks–Mecking diagram [29], is the diminishing of stages III and IV
with increasing pass number. After applying second pass, stage IV
is completely eliminated and stage III is only limited to small range
of stress before occurring plastic instability. Since with increasing
pass number, uniform elongation is decreased, therefore stages of
work hardening are decreased. As a result, for three passes CGPed
sheet, one stage of work hardening is acceptable.
Fig. 9. Hall–Petch relations for YS data of CGPed 1100 [9] and 3003 alloys.
 F. Khakbaz, M. Kazeminezhad / Journal of Manufacturing Processes 14 (2012) 20–25
Fig. 10. Work hardening rate versus true stress for different grain sizes
(Kocks–Mecking diagram).
4. Conclusions
A non-hardenable aluminum alloy 3003 was successfully sub-
jected to severe plastic deformation by CGP process. Results show
the effectiveness of this process in grain refinement and strength
improvement. After third pass of process, grain size of 580 nm is
achieved, and also mechanical properties of studied alloy are dras-
tically enhanced 170% in comparison with those of annealed sheet.
Improvement in mechanical properties is due to high rate of work
hardening which arises from fine dispersoids of Al6 Mn. Presence of
such particles can accelerate the rate of improvement in mechani-
cal properties and grain refinement, but in higher number of passes
these particles expedite effect of dynamic recovery and cease the
rate of mechanical properties improvement which investigations
on work hardening by a model based on dislocation density prove it.
Also, the results illustrate that the work hardening stages of Al–Mn
alloy are decreased with increasing strain or pass number.
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.
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