Materials Science & Engineering A 760 (2019) 7–18

Contents lists available at ScienceDirect

Materials Science & Engineering A

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

Development of combined groove pressing and rolling to produce ultra-fine T

grained Al alloys and comparison with cryorolling
Kandarp Changelaa, Hariharan Krishnaswamyb, Ravi Kumar Digavallia,∗
a
Department of Mechanical Engineering, Indian Institute of Technology Delhi, New Delhi, 110016, India
b
Department of Mechanical Engineering, Indian Institute of Technology Madras, Chennai, 600036, India

ARTICLE INFO ABSTRACT

Keywords: In the present work, aluminium alloys were subjected to two different severe plastic deformation (SPD) routes
Cryorolling namely, cryorolling (CYR) and constrained groove pressing (CGP), to investigate their effect on microstructure
Constrained groove pressing and mechanical properties. Solutionized AA 5083 alloy and AA 6061 alloy sheets were cryorolled to a final
Ultra-fine grains thickness of 1 mm with a total logarithmic strain of 1.87. Samples of these alloys with 3 mm thickness were
Dislocation density
subjected to CGP with an equivalent plastic strain of 1.16. The CGP samples have been subsequently cold rolled
(CR) to reduce the thickness to 1 mm (67% reduction). The microstructure of the deformed samples was
characterized by electron backscatter diffraction (EBSD) coupled with kernel average misorientation (KAM) and
X-ray diffraction (XRD). The techniques were employed to investigate the degree of grain refinement and local
misorientation due to deformation. It has been found that the yield strength (YS) of 6061 alloy after CGP + CR is
19% higher than that of CYR sample while, in contrast, the YS of CGP + CR 5083 alloy is 18% less than that of
CYR condition. A dislocation density-based model has been used to estimate the sub-structural changes during
processing. The theoretical dislocation density estimated using the model agreed well with the experimental
values of both the alloys with a difference of about 2.5% in the case of 5083 and 6.5% in the case of 6061. It is
inferred from the analysis that the dislocation bow out is the predominant mechanism in both the materials.

1. Introduction
Aluminium alloys are extensively used for structural and functional
applications in the form of sheets and plates in automobile, aerospace
and marine industries. Heat treatable 6xxx and non-heat treatable 5xxx
aluminium alloys exhibit superior mechanical properties such as high
fatigue strength, strength to weight ratio, and corrosion resistance
[1,2]. They are cost effective when compared to 2xxx and 7xxx alu-
minium alloys. One of the major drawbacks of aluminium alloys in a
commercial application is their lower strength in comparison with low
carbon steel [3]. In the recent past, this has been addressed by produ-
cing ultra-fine grained (UFG) materials through severe plastic de-
formation (SPD) [4]. Ultra-fine grained (UFG) materials (grain size in
the range of 100 nm - 1 μm), owing to their excellent strength and
toughness, are suitable for the next generation of metals and alloys.
Table 1 shows the terminology of metallic materials in terms of their
average grain size.
Severe plastic deformation is an advanced material processing
technique imparting large plastic strain to the workpiece. The micro-
structure of these highly deformed metals can evolve with plastic
deformation due to high internal strain, dislocation density, and in-
creased grain boundary region with high-energy state [5]. Different
SPD techniques have been developed to produce ultra-fine grained
materials, especially from light metals such as aluminium alloys. Some
of the established SPD processes are Equal Channel Angular Pressing
(ECAP) [6], High-Pressure Torsion (HPT) [7], Accumulative Roll
Bonding (ARB) [8], Cryorolling (CYR) [9] and Constrained Groove
Pressing (CGP) [10]. All the processes are capable of developing dense
bulk sub-crystalline solids through significant microstructural refine-
ment. ECAP, HPT, and ARB have limitations such as high load, rela-
tively small final product, limited scalability, and high cost. In addition
to that, the saturation of grain refinement at large strain is a serious
issue during SPD processes [11] and is attributed to fixed deformation
conditions such as strain rate, strain path, and deformation tempera-
ture. It has also been observed that grain refinement can be enhanced
by changing the deformation conditions. Among the above-mentioned
SPD techniques, ARB, cryorolling, and CGP are capable of producing
UFG structure in sheet form. Therefore, a more detailed review of
cryorolling and CGP is presented here.

∗
Corresponding author.
E-mail address: dravi@mech.iitd.ac.in (R.K. Digavalli).

https://doi.org/10.1016/j.msea.2019.05.088
Received 9 March 2019; Received in revised form 21 May 2019; Accepted 22 May 2019
Available online 24 May 2019
0921-5093/ © 2019 Published by Elsevier B.V.
K. Changela, et al.
Table 1
Range of average grain size with the corresponding terminology.
Terminology of metallic materials Average grain size
Amorphous 1 nm to ≤10 nm
Nanostructured 10 nm to ≤100 nm
Ultra-fine grain (UFG) 100 nm to ≤1 μm
Fine grain 1 μm to ≤10 μm
Coarse grain 10 μm–100 μm
1.1. Cryorolling
In cryorolling of Al and Cu alloys, it is possible to produce UFG
sheets by deformation at extremely low temperature which suppresses
the dynamic recovery and enhances the dislocation density by athermal
(work) hardening [12]. Wang et al. [9] initially performed cryorolling
on pure Cu up to a logarithmic strain of 2.3 and obtained high strength
UFG materials with sufficient ductility. Lee at al [13]. investigated the
effect of annealing temperature on the mechanical properties and mi-
crostructure of cryorolled AA 5083 alloy. The study indicated that op-
timizing the cryorolling, and subsequent annealing can yield high
strength to ductility ratio and equiaxed grains in the order of < 200 nm
with elongated subgrains. Panigrahi et al. [14] studied the aging
treatment of cryorolled AA6063 alloy and showed improved strength
and ductility compared to a cold rolled sample. Panigrahi and Jaya-
ganthan [15] studied the microstructural evolution at different strain
levels for this precipitation hardenable alloy. Marnette et al. [16]
showed that cryorolled pure aluminium samples exhibit a 30% higher
tensile strength than room temperature rolled samples. The stacking
fault energy (SFE) in metallic materials plays an important role in the
strengthening of cryorolled samples [17]. Significant improvement in
strength is reported in low SFE materials, whereas the improvement
was less than 10% in high SFE materials such as Al alloys and Ni
[18–20]. Wang et al. [9] showed that cryorolled and annealed pure Cu
with low SFE resulted in a bimodal grain structure with fine grains
embedded in a matrix of ultrafine grains due to the low driving force for
recrystallization. Recently, Feyissa et al. [21] reported a similar bi-
modal grain structure in AA 5083 alloy. Many researchers [18,22]
highlighted that cryorolling is a continuous processing route by which
UFG structure can be produced by imparting less plastic strain com-
pared to other SPD processes. However, one of the major drawbacks of
cryorolling is that the samples need to be treated in liquid nitrogen
atmosphere between successive passes resulting in higher processing
time. In addition to that, it has been reported that the difference in
strength improvement between cryorolling and cold rolling is marginal
[22].
1.2. Constrained groove pressing (CGP)
Shin et al. [10] have initially developed constrained groove pressing
technique. In this process, the blank is alternately pressed between
grooved and flat dies under plane strain condition. Each pass consists of
four stages, two in the grooved die and two in the flat die with a ro-
tation of 180° after two stages. The material is subjected to pure shear
deformation along the grooves. Zrnik et al. [23] investigated the CGP
process in commercially pure Al plate. The study revealed that the
microstructure after four successive passes consists of a severely banded
structure with equiaxed subgrains, of 1 μm size. However, the authors
observed that the microstructure after four passes was similar to that of
the first pass, which is due to the dynamic recovery and polygonization
in the deformed structure. A marginal drop in strength was observed by
Satheesh Kumar et al. [24] in pure nickel sheet after three passes of CGP
along with slight improvement in strain hardening ability and uniform
elongation. Khakbaz and Kazeminezhad [25] observed that the grain
refinement becomes inefficient after the third pass, and grain size was
approximately constant after the fourth pass with a steady-state
8
Materials Science & Engineering A 760 (2019) 7–18
microstructure. The rate of refinement was reduced due to dynamic
recovery. Peng et al. [26] reported that partially constrained CGP
process reduce the equivalent strain by 40% with respect to the fully
constrained condition when deforming H62 brass sample. Khoda-
bakhshi et al. [27] studied the CGP of low carbon steel and concluded
that after one pass, inhomogeneity in the sample increased compared to
the initial material.
From the above discussion, it can be concluded that the CGP process
is versatile and can be used for microstructural refinement in a wide
range of metallic materials. However, CGP process is known to impart
non-uniform deformation. The inherent geometric inhomogeneity in
the samples due to repeated grooving and flattening in the CGP sample,
which eventually leads to strain localization [28]. Yoon et al. [29]
observed that strain localization tendency increased with CGP passes
and is mainly due to non-uniform shear deformation along the sample
length. It is difficult to characterize the CGP sample with geometric
inhomogeneity that may have a non-uniform thickness in the transverse
direction [30]. In addition to that, this heterogeneity is closely related
to the level of grain refinement during the CGP process. It is therefore
essential to ensure uniform and consistent grain refinement when fi-
nalizing the process parameters in the SPD process.
In the present work, a new SPD route is proposed by combining
constrained groove pressing (CGP) and cold rolling (CR). Initially, the
samples are deformed for one pass by CGP, after which, they are cold
rolled at room temperature. This new processing route (CGP + CR) has
the potential to overcome the disadvantages of both CGP and cryorol-
ling. Both the CGP and CR are performed at room temperature, elim-
inating the need to soak in liquid nitrogen as required in cryorolling.
The subsequent cold rolling improves the surface flatness that can al-
leviate the geometric inhomogeneity as a result of the CGP process.
Recent work [31] showed that further rolling of severely deformed
samples imparts a higher plastic strain and results in ultra-fine grain
structure. The new SPD route is evaluated using solutionized AA 5083
and AA 6061 alloys. The mechanical properties and microstructure
from the proposed route (CGP + CR) are compared with cryorolling
(CYR) for similar sample thickness. A dislocation density based model is
used to discuss the microstructural characteristics of the processed
samples.
2. Experimental procedure
2.1. Materials and processing
The chemical composition of AA 5083 (‘O’ temper) and AA 6061
(‘T6’ temper) alloys used in the present study (as determined by spark
emission spectroscopy) is listed in Table 2.
The initial thickness of AA 5083 and AA 6061 was 6.5 and 3 mm,
respectively. The samples were cut to 100 mm × 200 mm, and
108 mm × 108 mm for cryorolling and constrained groove pressing,
respectively. The samples were solution treated at 530 °C for 2 h in a
muffle furnace followed by water quenching (as per ASTM B918M). The
solutionized (SL) samples were subjected to cryorolling (CYR) and
constrained grove pressing (CGP).
Cryorolling was performed after immersing the sample in a liquid
nitrogen bath for 30 min. During successive passes, the material was
immersed for sufficient time (at least 10 min) in liquid nitrogen to at-
tain stable temperature. Fig. 1 illustrates the cryorolling process sche-
matically. A four-high rolling mill with a roll diameter of 142 mm was
Table 2
Chemical composition of AA 5083 and AA 6061 alloys (wt %).
Alloy Mg Si Mn Cr Cu Fe Ti Zn Al
AA5083 4.73 0.128 0.670 0.053 0.015 0.222 0.046 0.028 94.108
AA6061 0.900 0.670 0.112 0.095 0.216 0.243 0.019 0.012 97.70
K. Changela, et al.
Fig. 1. Schematic of the cryorolling process using a four high rolling mill.
employed in the present work. A constant roll velocity of 14 m/min was
applied. The reduction per pass was restricted to around 4% to mini-
mize the temperature rise during rolling. Around 40 passes were ap-
proximately applied. The gap between the rollers was adjusted using a
pressure operated hand wheel. Around ∼ 85% reduction (from 6.5 mm
to 1 mm), corresponding to a logarithmic strain of 1.87 was applied to
the sample.
Constrained groove pressing experiments were carried out on a 300-
ton single action hydraulic press at room temperature. The applied load
was in the range of 60–70 tons. The CGP dies, and groove geometry
used in the present study is shown in Fig. 2. The width and height of the
corrugating indents of the grooved die are equal to the sheet thickness.
The groove angle and corner radius are 45° and 0.8 mm, respectively.
Each CGP pass induces an effective logarithmic strain of 1.16 [10].
The samples processed by CGP were cold rolled with a rolling di-
rection parallel to the grooves, and the final thickness was reduced to
1 mm (67% reduction with a logarithmic strain of 1.09). The schematic
Fig. 2. CGP dies used in the present study with groove geometry.
9
Materials Science & Engineering A 760 (2019) 7–18
illustration of the complete route for CGP followed by cold rolling is
presented in Fig. 3.
2.2. Characterization
2.2.1. Microstructure
Electron Back Scatter Diffraction (EBSD) and X-ray diffraction
(XRD) techniques were used to study the evolution of microstructure
and dislocation density. The samples for characterization were ex-
tracted from the center of the rolled sheet. The samples were polished
by standard metallographic procedure up to 3000 grit emery paper and
then polished with 3 μm and 1 μm diamond paste for mirror finish
followed by electropolishing at −15°C and 15 V DC using an electrolyte
of methanol: perchloric acid (80:20). EBSD analysis was performed on a
FEI, Quanta 3d FEG using TSL-OIM software. A step size of 0.1 μm was
used during the scan. XRD analysis was carried by Rigaku machine
using Cu Kα radiation with a scan speed of 2°/minute. The full width at
K. Changela, et al.
Fig. 3. Schematic illustration of CGP followed by cold rolling process.
half-maximum (FWHM) analysis was used to estimate crystallite size,
lattice strain, and dislocation density. The measured diffraction profile
is the convolution of physical broadening and instrumental broadening
profile. To subtract the instrumental broadening effect from the mea-
sured diffraction, Cauchy-Cauchy function can be employed as follows
[32]:
Bsample = Bexp Binst (1)
where Bsample , Bexp and BInst are actual sample broadening, experimental
broadening, and instrumental broadening, respectively. In this study,
instrumental broadening was corrected by measuring the peaks under
the identical condition from a fully annealed pure aluminium. FWHM
(B) were calculated using PANalytical X'pert High score software.
2.2.2. Mechanical properties
Hardness and tensile tests were carried out to investigate the me-
chanical properties. The samples were tested immediately after pro-
cessing to prevent natural aging. The hardness was measured using a
Vickers hardness tester by applying a load of 10 kg for 10 s dwell time.
An average of 10 measurements was taken at multiple locations parallel
to the rolling direction. In CGP samples, the hardness was measured on
the thickness plane along the transverse direction (perpendicular to
groove) at different locations with a gap of 5 mm. The standard tensile
properties such as yield strength, ultimate tensile strength and total
elongation of solutionized and deformed samples were determined by
uniaxial tensile tests. The tensile samples were cut along the rolling
direction for CYR and CGP + CR samples and parallel to groove di-
rection for CGP samples as per ASTM standard E8M. The tests were
conducted at room temperature at a constant crosshead speed of
1.92 mm/min with an initial strain rate of 10 3 s 1 on an INSTRON 5582
machine with a video extensometer. For each processing condition, five
samples were tested to ensure the repeatability of results. The yield
strength was determined using a 0.2% offset method. True stress-
logarithmic strain curves were plotted assuming Hollomon strain-
hardening law, = K n where, n is strain hardening exponent and, K
is the strength coefficient.
3. Results and discussion
3.1. Microstructure
The orientation image micrographs (OIM) obtained from EBSD
analysis are shown in Fig. 4. The corresponding misorientation dis-
tributions of grains or subgrains are shown in Fig. 5. The microstructure
of SL 5083 (Fig. 4a) shows equiaxed grains with an average size of
22 μm. The grains were difficult to distinguish in the severely deformed
structure in the CYR sample (Fig. 4b). The deformed microstructure
revealed diffused and ill-defined low angle grain boundaries due to
severe fragmentation of grains. The misorientation distribution of SL
5083 alloy shows a high fraction of high angle grain boundaries
(HAGBs) (Fig. 5a) while in CYR samples, a high fraction of low angle
grain boundaries (LAGBs) are observed. The latter is attributed to the
10
Materials Science & Engineering A 760 (2019) 7–18
fine dislocation structures within the grains. Similar results were re-
ported by Dhal et al. [33] in the cryorolled Al alloy with a 97% re-
duction. They observed that the dislocations accumulate and rearrange
themselves inside the grains resulting in LAGBs due to misorientation of
crystallites within the grains.
Fig. 4c and d show the OIM maps of AA 6061 alloy in solutionized
and cryorolled condition, respectively. The SL sample shows equiaxed
coarse grains with an average size of 88 μm and CYR 6061 micro-
structure consists of fine elongated grains parallel to rolling direction
with a low aspect ratio. The microstructure is similar to CYR 5083
samples. The microstructure of SL 6061 shows predominantly high
angle grain boundaries (88%), as shown in Fig. 5c while after cryor-
olling, a high fraction of low angle grain boundaries (93%) are formed.
Fig. 4e shows the microstructure of 6061 alloy after one CGP pass.
Grain refinement with an average grain size of 18 μm was observed.
Black arrow indicates that grains are severely banded and shattered due
to a high degree of shear stresses. Two different types of grains can be
seen in the microstructure. Equiaxed coarse grains with an average size
of 25 μm are seen in the region (A) of the sample while smaller, and
elongated grains with an average size of 12 μm are observed in the
region (B) indicating a non-homogenous structure. The distribution of
non-homogeneous structure in the transverse direction (perpendicular
to groove) of CGP sample after the first pass can be attributed to the
combined effect of geometric and strain inhomogeneity [30]. According
to Kumar et al. [34] and Yadav et al. [28], the corner region is subjected
to both shear strain and bending strain leading to fine grain structure
while the slant groove region, experiences only shear strain leading to
equiaxed coarse grains. The present results correlate with the above
observation. The inhomogeneity at the micro level was also detected in
the hardness measurements. Cold rolling of the samples subjected to
CGP of AA 6061 alloy shows a more refined microstructure and elon-
gated grains along the rolling direction (Fig. 4f). Black arrow indicates
the refined grains with an average size of < 1 μm. However, entire
microstructure with clear grain boundaries could not be seen in EBSD
pictures.
3.1.1. Kernel average misorientation (KAM) and dislocation structure
Kernel average misorientation (KAM) maps give a good estimation
of dislocation density and stored energy in the deformed materials.
KAM represents the average misorientation (within 5°) of each point
with respect to its neighboring points along the perimeter of the kernel
[35]. Fig. 5b and d show the KAM distributions of AA 5083 and AA
6061 alloy samples in SL and CYR conditions, respectively. As expected,
the KAM value of CYR 5083 sample (1.37) is approximately three times
more than the SL 5083 sample (0.45). The distribution of KAM in CYR
5083 samples is comparatively broader (higher KAM value) than SL
5083. According to Zhong et al. [36], the KAM value correlates directly
with the dislocation density. Large KAM value can be seen at grain
boundary as well as within some grains, which represents hard crystal
orientation with low energy dislocation pattern. In addition to that,
KAM peak in CYR 5083 sample is spread towards higher angle, in-
dicating severe strain in the microstructure. Similar results were
K. Changela, et al.
Fig. 4. Typical EBSD orientation map analysis of aluminium alloys in different conditions (a) 5083 SL, (b) 5083-CYR, (c) 6061-SL, (d) 6061-CGP, (e) 6061- CGP (one
pass) and (f) 6061- CGP + CR.
reported by Kumar et al. [37] in cryorolled 6082 Al alloy. The KAM
value of CYR 6061 is 1.14 (Fig. 5d), which is slightly lower than that of
CYR 5083. It is mainly due to the low strain-hardening rate observed
during tensile deformation in the CYR 6061.
Kernel average misorientation (KAM) maps of SL and CYR 5083 are
shown in Fig. 6a and b, respectively. EBSD-KAM maps for SL and UFG
materials were obtained by using a step size of 0.3 μm and 0.1 μm,
11
Materials Science & Engineering A 760 (2019) 7–18
respectively. In SL 5083 sample, the local strains are homogeneously
distributed while KAM maps of CYR sample shows large misorientation
inside the grains. CYR samples of Al alloy, which is expected to have
high dislocation density, generally form dislocation subcells at large
strain. Dhal et al. [33] discussed that the dislocation climb velocity in
Al alloy is low when compared to pure Al due to limited dislocation
interaction attributed to the combined effect of medium staking fault
K. Changela, et al.
Fig. 5. Misorientation distribution (a, c and e) and KAM distribution (b, d and f) in AA 5083 and AA 6061 alloys in different processing conditions.
energy and solid solution strengthening. Dislocation multiplication
within the grains leads to tangled microstructure during low-tempera-
ture deformation. Green color shows a large amount of dislocation
accumulated in the material. The KAM maps for cryorolled samples are
denser than the solution treated samples, as indicated by Fig. 6a–d.
Fig. 6d–f compares the KAM maps of AA 6061 alloy in CYR, CGP, and
CGP + CR sample conditions. The KAM map after one pass CGP shown
in Fig. 6e indicates dislocation rich regions along the prior existing
grain boundaries and certain region within the grains. The dislocations
generated during plastic deformation can be divided into geometric
necessary dislocations (GNDs) and statistically stored dislocations
(SSDs). The GNDs are generated due to the strain gradient during non-
homogeneous deformation [38]. The formation of the banded structure
during CGP process could be due to the inhomogeneous distribution of
dislocation with high local dislocation density indicating a large
amount of GNDs generated. Although the distribution of dislocation is
much stronger than the solution treated sample (Fig. 5c), the con-
centrated green regions are significantly lower than the CYR sample
indicating lesser grain refinement in CGP (one pass). When the CGP
sample is further cold rolled, the KAM distribution (Figs. 5f and 6f) is
approximately similar to that of CYR 6061. Heavily rolled materials
12
Materials Science & Engineering A 760 (2019) 7–18
(CYR and CGP + CR) are expected to have elongated grains with
subgrains of high dislocation density. These heavily deformed struc-
tures are difficult to index through EBSD analysis. Therefore, X-ray
diffraction technique has been used to estimate the microstructural
details like crystallite size, lattice strain, and dislocation density for
deformed samples.
3.2. Grain refinement and dislocation density
Grain size, lattice strain, and dislocation density were estimated
using the Williamson–Hall equation which is given below
Bcos = 2 sin + K /D (2)
where B is the peak broadening, is the Bragg angle, is the lattice
strain, K is the Scherrer constant (0.94), is the wavelength of X-ray
used (1.54 A ) and D gives the grain size. Bcos θ is plotted against sin θ
using a linear fit, and the intercept and slope give the grain size and
lattice strain, respectively. In the present study, XRD peak analysis was
employed to obtain the microstructural details of deformed samples.
The XRD peaks obtained in the case of CYR, CGP, and CGP + CR
samples are shown in Fig. 7. The value of dislocation density was cal-
culated using the following Eqs. (3)–(5), which is related, to the
K. Changela, et al. Materials Science & Engineering A 760 (2019) 7–18

Fig. 6. KAM maps of (a) 5083-SL (b) 5083-CYR (c) 6061-SL (d) 6061-CYR (e) 6061- CGP (one pass) and (f) 6061- CGP + CR.

measured grain size, and lattices strain [32]. of FWHM analysis for a wider range of grain size, typically above
100 nm is not completely reliable. In the present work, the trend of
= D x (3)
s
variation of crystallite size measured using FWHM analysis is assumed
where D and s represents the dislocation density due to grain size and to correlate with the grain size variation.
due to strain broadening, respectively. The high-intensity peaks for all deformed condition show preferred
orientation along the corresponding slip plane, and this is attributed to
3
= the accumulation of lattice strain in the rolling direction. This shows
D
D2 (4)
that a strong texture is obtained during the SPD process. The crystallite
K 2 size decreased to 190 nm after cryorolling in the case of 5083, which is
= much smaller than the grain size in solutionized condition (22000 nm).
s
b2 (5)
A similar trend is observed for CYR 6061 alloy. It may also be perceived
where K= 6 , ε is the lattice strain and b is the Burgers vector = a/ 2 from Table 3 that the CGP followed by cold rolling exhibits severe grain
where a is the lattice parameter which is calculated from XRD. Table 3 refinement with enhanced dislocation density. The dislocation density
shows the grains size, lattice strain, and dislocation density of SL and all increased significantly after CYR and CGP + CR. The increase in dis-
deformed condition samples. It is found that the grain size of CYR and location density from SL to deformed samples in 5083 is higher (order
CGP + CR samples reduced with enhanced lattice strain and dislocation of 1013 to 1014) than that of 6061 alloys (1012 to 1013). It is consistent
density when compared to the SL and CGP samples. This refinement is with KAM maps discussed in the previous section 3.1.1. Similar results
the major effect of severe straining. Grain refinement can be confirmed were reported by Naga Krishna et al. [39] for cryorolled Al–Cu alloy
by the EBSD micrographs presented in Figs. 4 and 5. However, the use

13
K. Changela, et al. Materials Science & Engineering A 760 (2019) 7–18

Fig. 7. XRD patterns of CYR, CGP and CGP + CR samples of (a) 5083 and (b) 6061.

and Krishna et al. [40] for cryorolled AA 8090 alloy.

3.2.1. Prediction of dislocation density by dislocation bow out (Frank-Read

source) model
It is widely accepted that the Hall-Petch relationship for coarse
grain materials could be described by dislocation pile-up model [41].
Dislocation pile up model is suitable for coarse grain materials and less
sensitive to the UFG materials [42]. Ultra-fine grained materials may
invoke other deformation mechanisms and cannot be successfully de-
scribed using the classical Hall-Petch law [43]. Therefore, dislocation
bow out model has been used to determine the dislocation density of
UFG Al alloys in the present study. In this model, the motion of perfect
dislocation through grain and grain boundaries controls plastic de-
formation in the UFG material. These perfect dislocations are emitted
from grain boundaries and sheared through grains. Kato et al. [44]
discovered that number of pinning points lie on a slip plane at the grain
boundary, which acts as obstacles, and it is easy for the dislocations to
bow out through these obstacles. The dislocation bow-out is enabled by
the large network of grain boundaries in UFG materials. The physical
meaning of dislocation bow out behavior is that the flow stress in UFG
material is controlled by the critical shear stress (CSS), c which is re-
quired to attain dislocation loop (based on Frank-Read source) with
semicircular configuration. Fig. 8 shows the schematic of dislocation
Fig. 8. Schematic illustration of dislocation bow out mechanism in UFG ma-
bow out mechanism in which, the grain boundaries are the source for
terial (black dots indicate pinning points).
the emission of perfect dislocations. The yielding is closely related to
the critical shear stress ( c) and is theoretically expressed by Eq. (6)
[45], dislocation structure [46,47].
Using Eq. (6) the yield strength ( y) of UFG material can be written
Gb 3 L as
c = 1 ln 1+
2 L (1 ) 2 b 2 (6)
y = 0 +M c (7)
where G is the shear modulus, b is the Burgers vector (0.286 nm for Al),
L is the average mean free path of the dislocations. is the Poison's where M is the Taylor factor (3.06) [48], which is the random or-
ratio. Mean free path of the dislocations (L) is equivalent to reciprocal ientation factor of polycrystalline material. 0 is the friction stress,
of the square root of dislocation density (ρ) in a random or organized which is 16.7 MPa for Al alloy. Using Eqs. (6) and (7), the mean free

Table 3
Grain size, lattice strain and dislocation density values of CYR, CGP and CGP + CR samples.
Condition Grain sizea (nm) Lattice strain (x 10−3) Dislocation density (m−2) - Experiment Dislocation density (m−2) - Model

5083 6061 5083 6061 5083 6061 5083 6061

SL 22000 88000 0.2 0.02 4.71 × 1013 5.25 × 1012 – –
CYR 190 310 4.67 0.9 6.50 × 1014 7.63 × 1013 1.80 × 1015 4.72 × 1014
CGP – 18000 4.7 1.8 8.36 × 1013 5.75 × 1013 – –
CGP + CR 231 277 4.54 1.2 5.16 × 1014 1.13 × 1014 1.18 × 1015 7.5 × 1014

a
In case of CYR and CGP + CR, it is crystallite size from XRD.

14
K. Changela, et al.
Fig. 9. Hardness values of (a) 5083 and (b) 6061 in different processing conditions.
path of dislocation (L) can be calculated from the yield strength for
coarse grain and UFG materials. The dislocation density estimated from
Eqs. (6) and (7) for UFG materials are shown in Table 3 and correlates
reasonably well with the experiments. In the case of 6061, the dis-
location density after CGP + CR is approximately 50% more than the
CYR condition. Similarly, in 5083 material, dislocation density after
CGP + CR decreased to 80% of the CYR condition. The ratio of theo-
retical dislocation density and experimental dislocation density of both
Al alloys in CYR and CGP + CR conditions are approximately the same.
The theoretical dislocation density estimated using the model agreed
well with the experimental values of both the alloys with a difference of
about 2.5% in the case of 5083 and 6.5% in the case of 6061. This
indicates that the dislocation bow-out is a dominant mechanism in CYR
and CGP + CR.
3.3. Mechanical properties
3.3.1. Hardness
Fig. 9 shows the variation in hardness values of samples of both the
alloys subjected to different processing conditions. The hardness in-
creased by 170 HV for CYR 5083, which is approximately 97% higher
than the SL sample (86 HV) while in CYR 6061, hardness increased
approximately by 155% higher than the SL sample (45 HV). However,
the difference in hardness between CYR (115 HV) and T6 (110 HV)
conditions is very less. The variation of hardness in the CGP and
CGP + CR samples for both Al alloys were evaluated by plotting
hardness against the distance in the transverse region (perpendicular to
the groove) in Fig. 10. The average hardness of the CGP 5083 sample
after four stages (ε = 1.16) is 130 HV which is 51% higher than the SL
condition while in CGP 6061 sample, hardness is approximately 104%
higher than the SL condition. A similar hardening behavior of pure Al
sample in one pass of CGP has been reported earlier [10]. It is seen in
Fig. 10 that in the SL sample, the hardness in the transverse direction is
approximately uniform, while in the CGP sample, the non-homogeneity
induces variation in the hardness distribution.
The variation of hardness along the transverse direction in the CGP
sample is due to the combined effect of geometric and microstructural
inhomogeneity. The inhomogeneity in CGP samples is drastically con-
trolled in the CGP + CR samples (Fig. 10). The photographs of CGP
processed samples after the first stage, the first pass, and cold rolling are
presented in Fig. 11. The CGP (first pass) sample portrays the im-
pressions of grooved marks formed on the sample during processing.
The cold rolling post CGP eliminated geometric inhomogeneity and
yielded improved hardness (Fig. 11).
15
Materials Science & Engineering A 760 (2019) 7–18
3.3.2. Tensile properties
The representative engineering stress-strain curves of all the sam-
ples are shown in Fig. 12 and the average mechanical properties are
summarized in Table 4. The yield strength (YS) and ultimate tensile
strength (UTS) of CYR 5083 sample, 450 MPa, and 530 MPa are higher
than SL condition (143 MPa and 282 MPa, respectively). A similar trend
is observed in the CYR 6061 sample also, in which yield strength in-
creased from 100 MPa to 274 MPa. The strengthening in CYR sample
can be attributed to two main reasons: (1) the grain refinement due to
suppression of dynamic recovery associated with climb and cross slip
and (2) higher dislocation density due to high plastic strain. However,
ductility and work hardening exponent (n) decreased due to lower work
hardening rate and inability to accumulate dislocations during sub-
sequent plastic deformation.
Work hardening exponent (n) and strength coefficient (K) of solu-
tionized and rolled samples are also shown in Table 4. The work
hardening exponent of rolled samples (CYR and CGP + CR) decreased
by 44–68% from the initial condition. The YS of CGP sample increased
by 40% and 82% for 5083 and 6061, respectively. The strength im-
provement after CGP in AA 5083 alloy is comparatively less than in AA
6061 alloy. The Portevin–Le Chatelier (PLC) effect in AA 5083 due to
dynamic strain aging (DSA) could be the possible reason for such
strength difference. The relatively higher Mg content in 5083 than 6061
alloy leads to appreciable PLC effect. The PLC effect is subsided in 6061
alloy as a major fraction of Mg in 6061 is present in the form of pre-
cipitates (as confirmed using XRD) [49] and not as solutes. Based on the
profile of PLC band, they can be classified as types A and B, wherein A
refers to smooth wavy band, and B refers to hopping bands with regular
stress drop [50]. As shown in Fig. 12, AA 6061 and AA 5083 alloys in SL
condition, exhibited type A and type B PLC band, respectively. The
maximum stress amplitude during dynamic strain aging was in the
order of 14 MPa in 5083 against 4 MPa in 6061 alloys. The stress drop
in type B bands observed in SL 5083 can lead to instability and pre-
mature strain localization. This strain localization can eventually lead
to premature failure and a reduced number of total passes. Hence,
AA5083 exhibits less improvement in strength compared to AA 6061
alloy after the CGP and CGP + CR process. The total elongation of CGP
sample decreased to more than two-thirds of SL condition. The me-
chanical behavior of CGP + CR samples is comparable to the CYR
samples. The strength increment in CGP + CR route is better than CYR
in AA 6061 alloy. Similarly, the loss of ductility in CGP + CR is lesser
than CYR samples. The ductility sharply decreased, which shows neg-
ligible strain hardening ability in CGP + CR samples. However, the
yield strength of CGP + CR 5083 sample increased by 62% from the
initial condition, which is less increased, compared to CYR 5083 (68%
increased) samples and UTS of the CGP + CR 5083 samples is 15% less
K. Changela, et al.
Fig. 10. Variation of hardness in transverse section of AA 5083 and AA6061 alloys in SL, CGP (one pass-perpendicular to groove direction) and CGP + CR conditions.
than CYR 5083 samples. It has been found that the yield strength (YS)
of 6061 alloy after CGP + CR is 19% higher than that of CYR sample
while, in contrast, the YS of CGP + CR 5083 alloy is 18% less than that
of CYR condition. The yield strength of CYR and CGP + CR 6061
samples is even higher than in T6 condition.
From the above discussion, it can be summarized that in 6061 al-
loys, both strength and ductility could be achieved by CGP + CR than
by CYR but in 5083 alloys, CYR sample has higher strength than in
CGP + CR method. The strengthening of 5083 alloy is significant
during the cryorolling process than CGP + CR process. It could be at-
tributed to the additional solid solution strengthening during cryorol-
ling as the solubility of Mg atoms in cryo conditions is unaffected by
atomic diffusion or recovery [51]. The reduced dislocation mobility
during cryorolling leads to localization and heterogeneous distribution
of dislocations.
4. Conclusions
The effect of two different severe plastic deformation (SPD) routes,
CYR, and CGP + CR on microstructure, dislocation density, and me-
chanical properties of AA 5083 and AA6061 alloys has been in-
vestigated in the present work. The following conclusions are drawn:
Fig. 11. Photographs of CGP processed AA 6061 alloy samples after the first stage, first pass and cold rolling.
16
Materials Science & Engineering A 760 (2019) 7–18
(1) The orientation image micrographs (OIM) revealed that the Al al-
loys in CYR and CGP + CR conditions exhibit elongated grains
along the rolling direction with a low aspect ratio. The average
misorientation distribution shows the formation of a high fraction
of low angle grain boundaries in these deformed samples, which is
attributed to fine dislocation structure within the grains.
(2) The kernel average misorientation (KAM) results indicate that the
homogeneous dislocation structure in SL condition changes to a
specific dislocation pattern with high dislocation density in the
deformed samples. In the case of 6061 alloys, KAM value of
CGP + CR sample is 1.16, which is 50% less than that of CGP
sample and is in similar order when compared to cryorolling.
(3) The high level of grain refinement during CYR and CGP + CR is a
major cause of high dislocation density. The predicted dislocation
density using dislocation bow out model correlates well with the
experimental values obtained from XRD analysis indicating dis-
location bow-out is the dominant mechanism in these two alloys.
(4) A significant improvement in the strength and hardness has been
observed after CYR, CGP (one pass) and CGP + CR. The CGP (one
pass) sample exhibits a non-homogeneous distribution of hardness
along the transverse direction, and it is mainly attributed to geo-
metric inhomogeneity induced by grooving dies and the
K. Changela, et al. Materials Science & Engineering A 760 (2019) 7–18

Fig. 12. Tensile stress-strain curves of Al alloys samples in different conditions (a) 5083 and (b) 6061.

Table 4
Mechanical properties of Al alloy samples in different conditions.
Condition YS (MPa) UTS (MPa) Total elongation (%) Work hardening exponent (n) Strength coefficient (K, MPa)

5083 6061 5083 6061 5083 6061 5083 6061 5083 6061
SL 143 ± 2 100 ± 3 282 ± 3 174 ± 2 25.2 ± 2.2 22.5 ± 1.1 0.3 ± 0.01 0.22 ± 0.01 544 ± 6 305 ± 8
T6 – 218 ± 3 – 317 ± 2 – 17.7 ± 0.1 – 0.18 ± 0.02 – 528 ± 5
CYR 450 ± 12 274 ± 5 530 ± 4 306 ± 3 6.35 ± 0.46 3.77 ± 0.24 0.14 ± 0.02 0.09 ± 0.04 862 ± 8 450 ± 9
CGP (1pass) 200 ± 20 182 ± 18 361 ± 8 262 ± 5 6.64 ± 0.74 6.13 ± 0.35 0.25 ± 0.09 0.19 ± 0.05 735 ± 12 530 ± 10
CGP + CR 380 ± 3 341 ± 8 460 ± 5 365 ± 5 3.5 ± 1.14 7.43 ± 0.42 0.17 ± 0.05 0.07 ± 0.02 866 ± 6 474 ± 8

microstructural inhomogeneity due to non-uniform grain refine-
ment. A further enhancement of both strength and ductility has
been achieved after the cold rolling of CGP sample in AA 6061 alloy
while the response to strengthening in AA 5083 alloy is significant
during cryorolling only. It is possibly due to the predominant oc-
currence of PLC bands (type B) restricting the strength improve-
ment in AA 5083 alloy during CGP.
(5) Overall, this study shows that CGP followed by cold rolling is a
suitable alternate route to produce the sheets of Al alloys with ultra-
fine grained structure and enhanced strength comparable to that of
cryorolled sheets.
Acknowledgment
Kandarp Changela acknowledges the assistantship received by
Ministry of Human Resource Development, Government of India during
his research work. Authors would like to acknowledge the help received
from Prof. I. Samajdar and researchers in his group at IIT Bombay for
microstructural characterization.
References
[1] S.M. Ashrafizadeh, A.R. Eivani, H.R. Jafarian, J. Zhou, Improvement of mechanical
properties of AA6063 aluminum alloy after equal-channel angular pressing by ap-
plying a two-stage solution treatment, Mater. Sci. Eng. A 687 (2017) 54–62.
[2] M. Samaee, S. Najafi, A.R. Eivani, H.R. Jafarian, J. Zhou, Simultaneous improve-
ments of the strength and ductility of fine-grained AA6063 alloy with increasing
number of ECAP passes, Mater. Sci. Eng. A 669 (2016) 350–357.
[3] D. Raja Satish, F. Feyissa, D. Ravi Kumar, Cryorolling and warm forming of AA6061
aluminum alloy sheets, Mater. Manuf. Process. 32 (2017) 1345–1352.
[4] R.Z. Valiev, R.K. Islamgaliev, I.V. Alexandrov, Bulk nanostructured materials from
severe plastic deformation, Prog. Mater. Sci. 45 (2000) 103–189.
[5] Z. Horita, D.J. Smith, M. Nemoto, R.Z. Valiev, T.G. Langdon, Observations of grain
boundary structure in sub micrometer- grained Cu and Ni using high-resolution
electron microscopy, J. Mater. Res. 13 (1988) 446–450.
[6] V.M. Segal, Equal channel angular extrusion: from macro-mechanics to structure
formation, Mater. Sci. Eng. A 271 (1999) 322–333.
[7] K. Edalati, Z. Horita, A review on high-pressure torsion (HPT) from 1935 to 1988,
Mater. Sci. Eng. A 652 (2016) 325–352.
[8] Y. Saito, N. Tsuji, H. Utsunomiya, T. Sakai, R.G. Hong, Ultra-fine grained bulk
aluminum produced by accumulative roll-bonding process, Scripta Mater. 39
(1998) 1221–1227.
[9] Y. Wang, M. Chen, F. Zhou, E. Ma, High tensile ductility in a nanostructured metal,
Nature 419 (2002) 912–915.
[10] D.H. Shin, J.J. Park, Y.S. Kim, K.T. Park, Constrained groove pressing and its ap-
plication to grain refinement of aluminum, Mater. Sci. Eng. A 328 (2002) 98–103.
[11] P.B. Prangnell, Y. Huang, The effect of cryogenic deformation on the limiting grain
size in an SMG Al-alloy, J. Mater. Sci. 43 (2008) 7280–7285.
[12] V. Parmar, K. Changela, B. Srinivas, M. Mani Sankar, S. Mohanty, S.K. Panigrahi,
K. Hariharan, D. Kalyanasundaram, Relationship between dislocation density and
antibacterial activity of cryo-Rolled and cold-rolled copper, Materials 12 (2019)
1–11.
[13] Y.B. Lee, D.H. Shin, K.T. Park, W.J. Nam, Effect of annealing temperature on mi-
crostructures and mechanical properties of a 5083 Al alloy deformed at cryogenic
temperature, Scripta Mater. 51 (2004) 355–359.
[14] S.K. Panigrahi, R. Jayaganthan, V. Pancholi, Effect of plastic deformation condi-
tions on microstructural characteristics and mechanical properties of Al 6063 alloy,
Mater. Des. 30 (2009) 1894–1901.
[15] S.K. Panigrahi, R. Jayaganthan, Development of ultrafine-grained Al 6063 alloy by
cryorolling with the optimized initial heat treatment conditions, Mater. Des. 32
(2011) 2172–2180.
[16] J. Marnette, M. Weiss, P.D. Hodgson, Roll-formability of cryo-rolled ultrafine alu-
minium sheet, Mater. Des. 63 (2014) 471–478.
[17] V. Subramanya Sarma, J. Wang, W.W. Jian, A. Kauffmann, H. Conrad,
J. Freudenberger, Y.T. Zhu, Role of stacking fault energy in strengthening due to
cryo-deformation of FCC metals, Mater. Sci. Eng. A 527 (2010) 7624–7630.
[18] S. Cheng, Y.H. Zhao, Y.T. Zhu, E. Ma, Optimizing the strength and ductility of fine
structured 2024 Al alloy by nano-precipitation, Acta Mater. 55 (2007) 5822–5832.
[19] T.R. Lee, C.P. Chang, P.W. Kao, The tensile behavior and deformation micro-
structure of cryo-rolled and annealed pure nickel, Mater. Sci. Eng. A 408 (2005)
131–135.
[20] D. Singh, P.N. Rao, R. Jayaganthan, Effect of deformation temperature on me-
chanical properties of ultrafine grained Al–Mg alloys processed by rolling, Mater.
Des. 50 (2013) 646–655.
[21] F. Feyissa, D.R. Kumar, P.N. Rao, Characterization of microstructure, mechanical
properties and formability of cryorolled AA5083 alloy, J. Mater. Eng. Perform. 27
(2018) 1614–1627.
[22] V.L. Niranjani, K.C. Hari Kumar, V.S. Sarma, Development of high strength Al-Mg-Si
AA6061 alloy through cold rolling and ageing, Mater. Sci. Eng. A 515 (2009)
169–174.
[23] J. Zrnik, T. Kovarik, Z. Novy, M. Cieslar, Ultrafine-grained structure development
and deformation behavior of aluminium processed by constrained groove pressing,
Mater. Sci. Eng. A 503 (2009) 126–129.
[24] S.S. Satheesh Kumar, T. Raghu, Tensile behaviour and strain hardening character-
istics of constrained groove pressed nickel sheets, Mater. Des. 32 (2011)

17
K. Changela, et al.
4650–4657.
[25] F. Khakbaz, M. Kazeminezhad, Work hardening and mechanical properties of se-
verely deformed AA3003 by constrained groove pressing, J. Manuf. Process. 14
(2012) 20–25.
[26] K. Peng, X. Mou, J. Zeng, L.L. Shaw, K. Qian, Equivalent strain, microstructure and
hardness of H62 brass deformed by constrained groove pressing, Comput. Mater.
Sci. 50 (2011) 1526–1532.
[27] F. Khodabakhshi, M. Kazeminezhad, H. Kokabi, Constrained groove pressing of low
carbon steel: nanostructure and mechanical properties, Mater. Sci. Eng. A 527
(2010) 4043–4049.
[28] P.C. Yadav, A. Sinhal, S. Sahu, A. Roy, S. Shekhar, Microstructural inhomogeneity
in constrained groove pressed Cu-Zn alloy sheet, J. Mater. Eng. Perform. 25 (2016)
2604–2614.
[29] S.C. Yoon, A. Krishnaiah, U. Chakkingal, H. Seop, Severe plastic deformation and
strain localization in groove pressing, Comput. Mater. Sci. 43 (2008) 641–645.
[30] S. Kumar, S. Venkatachalam, K. Hariharan, D.R. Kumar, H. Murthy, Influence of
inhomogeneous deformation on tensile behavior of sheets processed through con-
strained groove pressing, J. Eng. Mater. Technol. 141 (2019), https://doi.org/10.
1115/1.4043492.
[31] H. Pouraliakbar, M.R. Jandaghi, A. Heidarzadeh, M.M. Jandaghi, Constrained
groove pressing, cold rolling, and post-deformation isothermal annealing: con-
sequences of their synergy on material behavior, Mater. Chem. Phys. 206 (2018)
85–93.
[32] R.E. Smallman, K.H. Westmacott, Stacking faults in face-centered cubic metals and
alloys, Phil. Mag. 2 (2010) 669–683.
[33] A. Dhal, S.K. Panigrahi, M.S. Shunmugam, Insight into the microstructural evolu-
tion during cryo-severe plastic deformation and post-deformation annealing of
aluminum and its alloys, J. Alloy. Comp. 726 (2017) 1205–1219.
[34] S. Kumar, K. Hariharan, D.R. Kumar, S.K. Paul, Accounting bauschinger effect in the
numerical simulation of constrained groove pressing process, J. Manuf. Process. 38
(2019) 49–62.
[35] S. Goel, R. Jayaganthan, I.V. Singh, D. Srivastava, G.K. Dey, N. Saibaba, Texture
evolution and ultrafine grain formation in cross-cryo-rolled zircaloy-2, Acta Metall.
Sin. 28 (2015) 837–846.
[36] Y. Zhong, F. Yin, T. Sakaguchi, K. Nagai, K. Yang, Dislocation structure evolution
and characterization in the compression deformed Mn–Cu alloy, Acta Mater. 55
(2007) 2747–2756.
18
Materials Science & Engineering A 760 (2019) 7–18
[37] N. Kumar, S. Goel, R. Jayaganthan, G.M. Owolabi, The influence of metallurgical
factors on low cycle fatigue behavior of ultrafine grained 6082 Al alloy, Int. J.
Fatigue 110 (2018) 130–143.
[38] J.Q. Su, T.W. Nelson, T.R. Mcnelley, R.S. Mishra, Development of nanocrystalline
structure in Cu during friction stir processing (FSP), Mater. Sci. Eng. A 528 (2011)
5458–5464.
[39] N. Naga Krishna, R. Tejas, K. Sivaprasad, K. Venkateswarlu, Study on cryorolled Al-
Cu alloy using X-ray diffraction line profile analysis and evaluation of strengthening
mechanisms, Mater. Des. 52 (2013) 785–790.
[40] K.S.V.B.R. Krishna, M. Ashfaq, V. Varun, K. Sivaprasad, K. Venkateswarlu,
S.S.R. Akella, On plastic deformation behavior of cryorolled AA 8090 alloy, Trans.
Indian Inst. Met. 70 (2017) 1463–1475.
[41] H. Conrad, J. Narayan, Mechanisms for grain size hardening and softening in Zn,
Acta Mater. 50 (2002) 5067–5078.
[42] H. Conrad, Grain size dependence of the plastic deformation kinetics in Cu, Mater.
Sci. Eng. A 341 (2003) 216–228.
[43] R. Kapoor, J.K. Chakravartty, Deformation behavior of an ultrafine-grained Al-Mg
alloy produced by equal-channel angular pressing, Acta Mater. 55 (2007)
5408–5418.
[44] M. Kato, T. Fujii, S. Onaka, Dislocation bow-out model for yield stress of ultra-fine
grained materials, Mater. Trans. 49 (2008) 1278–1283.
[45] Y.G. Ko, D.H. Shin, K.T. Park, C.S. Lee, An analysis of the strain hardening behavior
of ultra-fine grain pure titanium, Scripta Mater. 54 (2006) 1785–1789.
[46] U.F. Kocks, H. Mecking, Physics and phenomenology of strain hardening: the FCC
case, Prog. Mater. Sci. 48 (2003) 171–273.
[47] D.L. Holt, Dislocation cell formation in metals, J. Appl. Phys. 41 (1970) 3197–3201.
[48] R.E. Stoller, S.J. Zinkle, On the relationship between uniaxial yield strength and
resolved shear stress in polycrystalline materials, J. Nucl. Mater. 283–287 (2000)
349–352 Part 1.
[49] M. Haghshenas, J.T. Wood, R.J. Klassen, Investigation of strain-hardening rate on
splined mandrel flow forming of 5052 and 6061 aluminum alloys, Mater. Sci. Eng.
A 532 (2012) 287–294.
[50] A. Yilmaz, The Portevin–Le Chatelier effect: a review of experimental findings, Sci.
Technol. Adv. Mater. 12 (2011) 1–16.
[51] J. Shi, L. Hou, J. Zuo, L. Zhuang, J. Zhang, A Cryogenic rolling-enhanced me-
chanical properties and microstructural evolution of 5052 Al-Mg alloy, Mater. Sci.
Eng. A 701 (2017) 274–284.