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Scripta Materialia 66 (2012) 911–914

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High-temperature deformation and structural restoration

of a nanostructured Al alloy
H. Asgharzadeh,a A. Simchib,c,⇑ and H.S. Kimd
a
Department of Materials Engineering, Faculty of Mechanical Engineering, University of Tabriz, P.O. Box 51666-16471, Tabriz, Iran
b
Department of Materials Science and Engineering, Sharif University of Technology, P.O. Box 11365-9466, Tehran, Iran
c
Institute for Nanoscience and Nanotechnology, Sharif University of Technology, P.O. Box 11365-9466, Tehran, Iran
d
Department of Materials Science and Engineering, Pohang University of Science and Technology, P.O. Box 790-784, Pohang,
South Korea
Received 14 November 2011; revised 9 February 2012; accepted 13 February 2012
Available online 24 February 2012

We studied the flow stress and microstructural changes of nanostructured Al-6063 alloy produced by mechanical alloying at var-
ious temperatures and strain rates. The analysis of flow curves was performed by a constitutive equation, and the stress exponent
and activation energy were determined as functions of strain. The deformation mechanisms were elaborated through microstructural
observations by electron backscattering diffraction and transmission electron microscopy. Coarsening of the subgrains and grain
growth upon deformation was monitored and related to the Zener–Hollomon parameter.
Ó 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Aluminum; Nanostructured materials; High-temperature deformation; Restoration mechanisms

Interest in the field of nanostructured (NS) mate-
rials has grown dramatically in the last decade due to
their unique microstructures and mechanical perfor-
mance [1]. Bulk NS metals are frequently produced by
severe plastic deformation (SPD) techniques, such as
equal channel angular extrusion [2], high-pressure
torsion [3] and mechanical milling followed by hot
consolidation methods [4]. NS materials exhibit higher
strength and lower ductility and formability compared
to their coarse-grained (CG) counterparts [5]. In
spite of significant studies on the room-temperature
properties of NS materials, their mechanical properties
at elevated temperatures, particularly restoration mech-
anisms involved in microstructural changes occurring
during the deformation, have been reported only rarely.
Horita et al. [6] and Park et al. [7] showed that the fine
grain structure of SPD-processed Al alloys could be
stable up to 300 °C (0.5Tm), whereas consistent grain
growth occurred at higher temperatures. Ma et al. [8]
observed superplastic behavior in an ultrafine-grained
Al alloy through grain boundary sliding. The deforma-
tion mechanism of NS aluminum alloys at elevated
⇑ Corresponding author at: Department of Materials Science and
Engineering, Sharif University of Technology, P.O. Box 11365-9466,
Tehran, Iran. Tel./fax: +98 21 6616 5262; e-mail: simchi@sharif.edu
temperatures may be controlled by dislocation climb
as well [9].
In general, NS materials have a large area of grain
boundaries and therefore a large stored energy, and are
intrinsically unstable with respect to grain growth during
the high-temperature deformation operation [10]. There-
fore, it is imperative and useful to study the deformation
behavior of NS materials and to determine the restora-
tion mechanisms dependent on temperature, strain and
strain rate. As a follow-up to our recent work on
room-temperature mechanical behavior of NS-Al6063
alloy [11], we herein report the microstructural evolution
of the alloy during high deformation at different temper-
atures and strain rates. The effects of thermomechanical
parameters on the flow behavior and dynamic restora-
tion mechanisms are presented and discussed.
Details of the processing method of the NS Al alloy can
be found in Ref. [12]. Briefly, gas-atomized Al-6063 pow-
der, with a chemical composition of Al–0.64Mg–0.67Si–
0.32Fe–0.2Cu (in wt.%), was utilized. Mechanical alloy-
ing was performed in an attrition ball mill (Union Process,
OH, USA) for 20 h under an Ar atmosphere. Stearic acid
(1.5 wt.%) was added as process control agent (PCA). The
powder was degassed at 400 °C, compacted in an alumi-
num container and finally extruded at 450 °C with an
extrusion ratio of 14:1. Cylindrical specimens with diam-
eter of 4 mm and an aspect ratio of 1.2 were machined

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http://dx.doi.org/10.1016/j.scriptamat.2012.02.026
912 H. Asgharzadeh et al. / Scripta Materialia 66 (2012) 911–914
from the extruded billet. Uniaxial compression test was
performed on a Caster and Thermomechanical Simulator
(Fuji Electronic Industrial Co., Ltd, Japan) under a high-
purity Ar atmosphere in a temperature of 300–450 °C and
a strain rate range of 0.01–1 s1. Quartz plates were used
for reducing the friction between the specimen and anvils.
A soaking time of 3 min at the testing temperature was
considered for temperature stabilization. To preserve
the microstructure after deformation, the specimens were
instantly quenched with a cooling rate of 70 °C s1.
The microstructural studies before and after defor-
mation were carried out by electron backscattering dif-
fraction (EBSD; Hikari, EDAX, NJ), using a field
emission gun scanning electron microscope (Helios
NanoLab DualBeam, FEI, Oregon), and transmission
electron microscopy (TEM; JEM-2100F STEM, Japan).
Figure 1 shows true stress–true strain curves of NS
Al-6063 at various temperatures and strain rates. The
true stress was corrected for friction according to the
slab analysis of the compression of a cylinder [13]. The
flow behavior dependent on the temperature and strain
rate is similar to that of CG aluminum alloy, as reported
elsewhere [14]. As seen, the flow stress expeditiously in-
creases to a maximum value and then gradually de-
creases with the true strain. This behavior is due to a
dynamic competition between the work hardening
caused by interaction, pile-up and tangling of disloca-
tions, and the work softening may be caused by dynamic
recovery (DRV), subgrain coarsening, dynamic precipi-
tation, dynamic recrystallization (DRX) and texture
softening [15].
The microstructural features of the alloy before and
after hot deformation at some selected conditions are
shown in Figure 2. In EBSD inverse pole-figure (IPF)
maps, low-angle boundaries (LABs) (misorientation be-
tween adjacent grains of 2°–15°) and high-angle bound-
aries (HABs) (misorientation larger than 15°) are shown
with white and black lines, respectively. The IPF image
of the as-extruded material reveals an elongated grain
structure with an aspect ratio of 2.9 (Fig. 2a). As shown
in Figure 2d, the microstructure consists of grains with a
wide size distribution in the ultrafine size range (>95%)
and an average value of 500 nm. While the microstruc-
ture consisted of a high fraction of HABs (fHAB  0.78),
some of the larger grains contain subgrains (Fig. 2a and
Figure 1. True stress–strain curves of NS Al-6063 alloy at various
temperatures and strain rates.
g). Consequently, a high value of the average misorien-
tation angle was measured (have  33°). Figure 2j
illustrates a representative TEM image of the micro-
structure. A high density of dislocations is observable
within larger grains while nanometric precipitates are
distributed in the microstructure. Figure 2b and c shows
that a significant change in the grain structure occurred
after hot deformation. The elongated grains were mainly
disappeared and nanostructured and ultrafine equiaxed
grains were formed after deformation at 300 °C and
1 s1 (Fig. 2b). The size distribution of grains became
narrower but the average grain size was slightly in-
creased (Fig. 2e). Moreover, the values of fHAB and have
were declined (Fig. 2h). To reveal the effect of tempera-
ture, the microstructure of the specimen deformed at
450 °C and 1 s1 is shown in Figure 2c. Micrometric
substructured grains and ultrafine equiaxed grains are
seen. Moreover, the grain size distribution is broader
(Fig. 2f) and the average grain size is coarser (760 nm).
Furthermore, a shift in the boundary misorientation dis-
tribution from high angles to low angles is noticed
(Fig. 2i). As a result, the values of fHAB and have changed
to 0.67 and 27°, respectively. Meanwhile, the stability of
precipitates during high-temperature deformation is
noticeable (Fig. 2k and l). The microstructural observa-
tions determine that DRV through the formation of
subgrains within the grains and DRX via formation of
recrystallized grains occurred during hot deformation
of NS Al-6063.
In order to determine the restoration mechanisms
involving in the deformation behavior, the following
hyperbolic sine law between the flow stress (r), temper-
ature (T) and strain rate (_e) was utilized [16]:
 
n Q
A½sinhðarÞ ¼ e_ exp ¼Z ð1Þ
RT
where Q is the deformation activation energy, R is the
gas constant, n is the stress exponent, Z is the Zener–
Hollomon parameter, and A and a are material con-
stants. The stress multiplier for the highest correlation
coefficient for the linear correlation between ln e_ and
ln sinh(ar) was determined to be a = 0.06 MPa1, which
is close to the value obtained for the CG Al alloys [16].
The values of n and Q at different strains (e) were deter-
mined from the slope of ln e_ vs. ln sinh(ar) plot and Rn
ln sinh(ar) vs. 1/T, respectively. An example of the pro-
cedure is shown in Supplementary Figure 3a and b for
e = 0.5. Figure 3 depicts the variation of activation en-
ergy and stress exponent with the true strain. Such
dependency has also been observed for a number of
CG Al alloys, such as AlFe8.5V1.3Si1.7 [17]. Data fitting
yields:
n ¼ 16:7e5  108 e4 þ 9:2e3 þ 3e2  4:7e þ 3:8 ð2Þ
Q ¼ 2441:7e5 þ 8:3e4 þ 1737:1e3  232:6e2  323:3e þ 298:4
ð3Þ
Although these equations are curve fitting expres-
sions and might not have a physical basis, an average
value of 2.9 ± 0.2 and 228 ± 21 kJ mol1 could be con-
sidered for n and Q, respectively, considering that the
variation of Q reflects changes in n, as explained else-
 H. Asgharzadeh et al. / Scripta Materialia 66 (2012) 911–914 913

Figure 2. Microstructural analysis of NS-Al6063 alloy before (left-hand-side images) and after deformation at 300 °C and 1 s1 (central images) and
450 °C and 1 s1 (right-hand-side images): (a–c) orientation maps from EBSD measurement (the insert in (a) shows a representation of the color code
used to identify the crystallographic orientations on standard stereographic projection); (d–f) grain size distribution from EBSD measurement; (g–i)
misorientation angle distribution from EBSD measurement; (j–l) TEM micrographs.

deformation. The higher activation energy can also be

Figure 3. Constitutive analysis of NS Al-6063 in hot compression.
Stress exponent (n) and activation energy (Q) as functions of true
strain (symbols and dashed lines show experimental data and the
polynomial fitted curves, respectively).
where [14]. Meanwhile, values in the range of 155–
205 kJ mol1 for the activation energy of CG Al–Mg–
Si alloys of various purities at pre-aged or annealed con-
ditions have been reported [16]. The higher activation
energy for the nanostructured Al-6063 can be attributed
to the microstructural features (nanostructured grains,
ultrafine grains and subgrains) that limit the cross slip
and climb processes, especially at the initial stages of
linked to the occurrence of DRX. The progressive accu-
mulation of dislocations in LABs increases their misori-
entation, leading to the transformation of LABs into
HABs. As the straining progresses, the subgrains, grains
and precipitates coalesce, easing dislocation motion so
that the activation energy falls (Fig. 3).
Figure 4a shows variation in the size of subgrains (dS)
and recrystallized grains (dR) as functions of ln Z.
Although lower values for dS and dR were obtained com-
pared to conventional Al alloys [18–20], these are com-
parable with those reported for SPD-processed Al
alloys with similar Z parameters [21]. Similar to CG
Al alloys [22], linear relationships in semi-logarithmic
scale can be established between the grain structure
and Z, i.e. d = a  b ln Z, where a and b are the fitting
parameters. The correlation of the dS and dR with the
steady-state flow stress (rss) in logarithmic scale is illus-
trated in Figure 4b. Similar to conventional alloys [23],
the graph shows that the relationship between the size
of subgrains and recrystallized grains with rss during
hot working can be expressed as rss = Kdm. However,
analysis of the data yielded m values of 2.56 and 1.04
for subgrains and recrystallized grains, respectively,
which are higher than those reported for the hot defor-
mation of micro-crystalline alloys [24,25].
914 H. Asgharzadeh et al. / Scripta Materialia 66 (2012) 911–914
Figure 4. Dependency of the size of subgrains and recrystallized grains
on (a) the Zener–Hollomon parameter and (b) the steady-state flow
stress.
The results indicate that significant changes in the
microstructure of the NS alloy occur during the hot
deformation, although fine particles are distributed in
the matrix (Fig. 2). As reported elsewhere [12], these
particles are mainly Al8Fe2Si, Al5FeSi and Al8Mg3Fe-
Si2, with a total of 1.8 vol.%. According to the theory
of Zener pinning, the volume fraction (Vf) of particles
with a diameter of dP required to stabilize a microstruc-
ture with an average grain size of D should be Vf = 4dp/
3D [1]. By considering dP = 62 nm [12], the required Vf
to stabilize the nanosize grains was estimated to be
16.5%. Therefore, effective grain boundary pinning can-
not be afforded by the particulates. It is pertinent to
point out that, upon mechanical milling and in the pres-
ence of PCA, carbides and oxides can be formed and
distributed within the Al matrix, and will contribute to
the dispersion strengthening [4,12]. We evaluated this ef-
fect by analyzing the threshold stress requiring for dislo-
cation motion at elevated temperatures [26] for NS Al-
6063 and obtained an approximate value of 1 MPa. This
observation reflects the minor influence of these parti-
cles, which have on the hot deformation behavior.
In conclusion, we studied the deformation behavior
and microstructural changes of a nanostructured Al-
6063 alloy across a wide range of temperatures and
strain rates. The stress exponent and activation energy
were correlated to strain with a fifth-order polynomial
curve. An apparent activation energy of
228 ± 21 kJ mol1 was obtained. The coarsening of the
subgrains, recrystallized grains and precipitates during
hot deformation, especially at low Z values, was shown.
Deformation at Z > 3.4  1017 s1 resulted in a refine-
ment of grain structure without a significant coarsening
of subgrains.
Supplementary data associated with this article can
be found, in the online version, at doi:10.1016/
j.scriptamat.2012.02.026.
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