metals

Article
Annealing Behavior of 6061 Al Alloy Subjected to
Differential Speed Rolling Deformation
Young Gun Ko 1 and Kotiba Hamad 2, *
1 School of Materials Science and Engineering, Yeungnam University, Gyeongsan 38541, Korea;
[email protected]
2 School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Korea
* Correspondence: [email protected]; Tel.: +82-31-290-7401

Received: 27 October 2017; Accepted: 6 November 2017; Published: 10 November 2017

Abstract: This study investigated the effects of heat treatment (annealing) on the microstructure
of ultrafine grained 6061 Al alloy samples fabricated by a differential speed rolling (DSR) process.
The samples were fabricated using two passes DSR with 75% thickness reduction and a speed ratio of 1:4.
The DSR-deformed 6061 Al alloy sample exhibited a lamellar boundary structure composed mostly of
subgrains surrounded by low-angle grain boundaries. After annealing, the DSR-deformed 6061 Al alloy
samples exhibited coarse grained structure and transformed from lamellar to equiaxed, where both the
grain size and grain shape aspect ratio increased with increasing annealing temperature. The fraction of
grain boundaries with high misorientation angles increased progressively during annealing, to ~77% at
annealing temperature of 350 ◦ C.

Keywords: differential speed rolling; 6061 Al alloy; annealing; microstructure

1. Introduction
The interest in ultrafine grained (UFG) materials with exceptional properties has increased rapidly
because of their scientific and technological importance. In recent studies, metals with an UFG
structure (mean grain size < 1 µm) showed extraordinary performance, such as improved strength
and low-temperature super-plasticity [1,2]. One method to achieve the UFG structure is severe
plastic deformation (SPD). Several methods have been applied successfully to fabricate UFG materials
using SPD. Those are equal-channel angular pressing (ECAP), accumulative roll bonding (ARB),
high pressure torsion (HPT) and differential speed rolling (DSR) [3–9]. Among them, DSR is the
method that shows a high capability to produce UFG sheets continuously. This is usually carried out
by imposing uniform shear strain in the thickness direction of the sheets through two identical rolls
with different rotation speeds [7–9].
Aluminum alloys are used for applications such as food packaging, sports utilities, automotive
and aircraft because of their high specific strength (strength/density ratio) and corrosion resistance.
Alloys with the base composition of ternary aluminum-magnesium-silicon, which are called 6xxx series,
possess good strength, heat-treatability, excellent formability and acceptable corrosion resistance [10].
In this series, 6061 Al alloy is the most commonly used alloy in many applications and can be
fabricated easily by extrusion, forging or rolling. To enhance the property of the 6061 Al alloy for
specific applications, grain refinement is used. Kim et al. [11] reported that the mechanical properties
of UFG 6061 alloy subjected to DSR deformation was higher than those fabricated by ECAP and HPT.
The excellent strength achieved after deformation by DSR is usually conjugated with the poor
ductility which has limited the material applicability in the industrial fields. For improving the strength
and ductility of the UFG materials, an appropriate thermal treatment following plastic deformation
is required. Several studies examining the effects of annealing have been carried out. Kim et al. [12]
reported that the thermal treatment of an ECAP deformed 6061 Al alloy was effective in improving

Metals 2017, 7, 494; doi:10.3390/met7110494 www.mdpi.com/journal/metals

Metals 2017,7,7,494
Metals2017, 494 22of
of10
10

Kim et al. [12] reported that the thermal treatment of an ECAP deformed 6061 Al alloy was effective
the strength whilst
in improving retaining
the strength moderate
whilst tensile
retaining ductility.
moderate Rezaei
tensile et al.Rezaei
ductility. [13] reported the
et al. [13] improved
reported the
performance (strength and ductility) of ARB-deformed sheets after a thermal treatment.
improved performance (strength and ductility) of ARB-deformed sheets after a thermal treatment. On the other
hand,
On thethere
otherhas beenthere
hand, no conclusive
has been no research on the
conclusive microstructural
research evolution of UFG
on the microstructural 6061 Al
evolution ofalloy
UFG
deformed by DSR during annealing. Therefore, the aim of this work is to investigate microstructural
6061 Al alloy deformed by DSR during annealing. Therefore, the aim of this work is to investigate
evolution of DSR-deformed
microstructural evolution of6061 Al alloy during
DSR-deformed 6061annealing.
Al alloy during annealing.
2. Experiments
2. Experiments
The chemical composition of the 6061 Al alloy sheets used in the present work was (in wt %):
The chemical composition of the 6061 Al alloy sheets used in the present work was (in wt %): 0.9
0.9 Mg, 0.71 Si, 0.5 Fe, 0.24 Cu, 0.19 Cr, 0.12 Mn, 0.05 Zn, 0.05 Ti, with Al comprising the balance.
Mg, 0.71 Si, 0.5 Fe, 0.24 Cu, 0.19 Cr, 0.12 Mn, 0.05 Zn, 0.05 Ti, with Al comprising the balance. The as-
The as-received sheets were cut into small plates, 0.4 cm (thickness), 4 cm (width) and 10 cm (length).
received sheets were cut into small plates, 0.4 cm (thickness), 4 cm (width) and 10 cm (length). The
The plates were then homogenized for 3 h at 550 ◦ C and air cooled to obtain a fully annealed structure
plates were then homogenized for 3 h at 550 °C and air cooled to obtain a fully annealed structure
(Figure 1). The homogenized plates were then subjected to the room-temperature DSR deformation
(Figure 1). The homogenized plates were then subjected to the room-temperature DSR deformation
using two identical rolls (220 mm in diameter). To impose the shear deformation by DSR, a speed
using two identical rolls (220 mm in diameter). To impose the shear deformation by DSR, a speed
ratio of 1:4 was used, where the lower roll speed was fixed to ~3 m/min. The plates were subjected
ratio of 1:4 was used, where the lower roll speed was fixed to ~3 m/min. The plates were subjected to
to two passes with 50% thickness reduction per pass, so that the total thickness reduction was 75%
two passes with 50% thickness reduction per pass, so that the total thickness reduction was 75% after
after the DSR deformation (two passes). During the DSR deformation, the plates were rotated by 180◦
the DSR deformation (two passes). During the DSR deformation, the plates were rotated by 180°
around their rolling direction between the adjacent passes. This route was found to be beneficial for
around their rolling direction between the adjacent passes. This route was found to be beneficial for
controlling the material with a fine grain structure [14,15]. The heat treatment was carried out on the
controlling the material with a fine grain structure [14,15]. The heat treatment was carried out on the
DSR-deformed plates for 1 h at various temperatures of 150–400 ◦ C with an interval of 25 ◦ C.
DSR-deformed plates for 1 h at various temperatures of 150–400 °C with an interval of 25 °C.

(a) (b)
Figure1.1.(a)
Figure (a)Homogenization
Homogenization conditions
conditions of
of the
the as-received
as-received 6061
6061 Al
Alalloy
alloysheets
sheetsand
and(b)
(b)the
theobtained
obtained
microstructure (DSR: Differential Speed Rolling; A.C.: Air Cooled).
microstructure (DSR: Differential Speed Rolling; A.C.: Air Cooled).

The structural features of the deformed and annealed plates were observed using electron
The structural features of the deformed and annealed plates were observed using electron
backscatter diffraction (EBSD, Hitachi S-4300 FESEM; Hitachi, Tokyo, Japan). For EBSD observations,
backscatter diffraction (EBSD, Hitachi S-4300 FESEM; Hitachi, Tokyo, Japan). For EBSD observations,
sample cut from the normal direction-rolling direction (ND-RD) plane, were electro-polished using
sample cut from the normal direction-rolling direction (ND-RD) plane, were electro-polished using
a solution of 20% perchloric acid in methanol at 25 V for 10 s. The EBSD observations were conducted
a solution of 20% perchloric acid in methanol at 25 V for 10 s. The EBSD observations were conducted
at a step size of 0.02 µm. The EBSD data was analyzed using a TSL OIM 6.1.3 (Hitachi, Tokyo, Japan)
at a step size of 0.02 µm. The EBSD data was analyzed using a TSL OIM 6.1.3 (Hitachi, Tokyo, Japan)
and the evaluation of misorientation distribution was made based on the assumption that the
and the evaluation of misorientation distribution was made based on the assumption that the
misorientation angles from 2° to 15° indicated the low angle-grain boundaries (LAGBs) whereas the
misorientation angles from 2◦ to 15◦ indicated the low angle-grain boundaries (LAGBs) whereas the
misorientation angles higher than 15° implied the high-angle grain boundaries (HAGBs).
misorientation angles higher than 15◦ implied the high-angle grain boundaries (HAGBs). Transmission
Transmission electron microscopy observations (TEM, Philips TECNAI G2F20; Drachten, The
electron microscopy observations (TEM, Philips TECNAI G2F20; Drachten, The Netherland) of the
Netherland) of the annealed plates were performed at an acceleration voltage of 200 kV. For this
annealed platesfoils
measurement, werecut performed at an acceleration
form the annealed plates were voltage
thinned of
by 200 kV. For
a focused ionthis measurement,
beam. To measure
foils
the Vickers microhardness, the annealed 6061 Al alloy plates with mirror-like surfaces the
cut form the annealed plates were thinned by a focused ion beam. To measure Vickers
were tested
microhardness, the annealed 6061 Al alloy plates with mirror-like surfaces were tested under
under a load and dwell time of 200 g and 10 s, respectively. In order to avoid the occurrence of naturala load
and dwell time of 200 g and 10 s, respectively. In order to avoid the occurrence
aging, the microstructure observations and hardness measurements were carried out right afterof natural aging,
the microstructure
deformation observations
and annealing and hardness measurements were carried out right after deformation
experiments.
and annealing experiments.
Metals 2017, 7, 494 3 of 10

Metals 2017, 7, 494 3 of 10

3. Results and Discussion
3. Results and Discussion
3.1. Microstructural Features of the Differential Speed Rolling-Deformed 6061 Al Alloy
3.1. Microstructural
Figure 2 shows theFeatures
EBSD ofmaps
the Differential
obtainedSpeed
fromRolling-Deformed
the near-surface 6061 Al Alloy
region of the 6061 Al alloy plate
deformedFigure
by the2 DSR
showsunder the investigated
the EBSD maps obtainedconditions (two passes,
from the near-surface 75%ofand
region 1:4).Al
the 6061 The EBSD
alloy platemaps
(inverse pole figure
deformed by the(IPF)
DSR and
undergrain boundaries conditions
the investigated (GBs)) in Figures 2a and
(two passes, 75%1b show
and 1:4).aThe
lamellar boundary
EBSD maps
(inverse
structure pole figure
composed (IPF) and
mostly grain boundaries
of subgrains (GBs))
with high in Figures
fraction 2a and 1b show
of low-angle graina lamellar boundary
boundaries (LAGBs),
structure composed mostly of subgrains with high fraction of low-angle grain
as shown by the dashed rectangle A in Figure 2a. In addition, a lower fraction of ultrafine boundaries (LAGBs),
grains
as shown by the dashed rectangle A in Figure 2a. In addition, a
◦ lower fraction
surrounded by boundaries with an angle of misorientation (>15 ) are also observed near the lamellarof ultrafine grains
surrounded by boundaries with an angle of misorientation (>15°) are also observed near the lamellar
boundaries (dashed rectangle B in Figure 2a). This was also confirmed by the grain boundaries map
boundaries (dashed rectangle B in Figure 2a). This was also confirmed by the grain boundaries map
presented in Figure 2b.
presented in Figure 2b.

Figure
Figure 2. (a)
2. (a) IPFIPF (InversePole
(Inverse Pole Figure),
Figure),(b)
(b)grain boundaries
grain and (c)
boundaries andpartitioned IPF maps
(c) partitioned of the
IPF DSR-
maps of the
deformed 6061 Al alloy.
DSR-deformed 6061 Al alloy.
The nucleation of such ultrafine grains around the elongated grains leads to a necklace-like
The nucleation
structure, which wasof such ultrafineingrains
also reported aroundafter
bcc materials thedeformation
elongated by grains
DSR leads to a necklace-like
at different thickness
reductions
structure, which[16,17].
was alsoThe reported
evolution in of bcc
the materials
necklace-like structure
after is typical
deformation byofDSR
a continuous
at different dynamic
thickness
recrystallization (CDRX) process at an intermediate stage of deformation by
reductions [16,17]. The evolution of the necklace-like structure is typical of a continuous dynamic SPD [18]. This can be
attributed to the rapid evolution of strain gradients near grain boundaries,
recrystallization (CDRX) process at an intermediate stage of deformation by SPD [18]. This can be leading to the formation
of large misorientations in the vicinities of the boundaries. Therefore, it is deduced that different grain
attributed to the rapid evolution of strain gradients near grain boundaries, leading to the formation of
refinement mechanisms can occur, depending on the materials and processing conditions.
large misorientations in the vicinities of the boundaries. Therefore, it is deduced that different grain
The fraction of ultrafine grains (~23%) in the deformed microstructure was determined by
refinement mechanisms
partitioning can grains
the ultrafine occur,using
depending on the
the criteria materials
of the and processing
grain orientation conditions.
spread (GOS) [19], as shown
The fraction
in Figure 2c. of
In ultrafine
addition, thegrains (~23%)layers
individual in theformed
deformed
betweenmicrostructure was determined
the lamellar boundaries were by
partitioning the ultrafine
characterized grainsgrain
by low-angle using the criteria
boundaries of theand
(LAGBs) grain orientation
intra-layer spreadgradients
orientation (GOS) [19], as shown
resulting
in Figure
in the 2c.
(sub)In addition,
grain theAfter
structure. individual layers formed
the DSR deformation, betweenofthe
the presence lamellar
LAGBs inside boundaries
the elongatedwere
grains is normally
characterized observed
by low-angle grainafter SPD deformation.
boundaries (LAGBs) Toand
explain the development
intra-layer of the
orientation (sub) grained
gradients resulting
in thestructure
(sub) graininside the individual
structure. Afterlayers,
the DSR thedeformation,
misorientationthe profiles were of
presence recorded
LAGBsalong inside thethe
rectangle
elongated
grainsAisinnormally
Figure 2a.observed
The misorientation
after SPDprofiles (point-to-origin
deformation. and the
To explain point-to-point)
development measured along grained
of the (sub) the
dashed line (L) are presented in Figure 3. The results showed large variation across the individual
structure inside the individual layers, the misorientation profiles were recorded along the rectangle
layer, where average values of 4.06° and 6.77° were recorded for point-to-origin and point-to-point
A in Figure 2a. The misorientation profiles (point-to-origin and point-to-point) measured along the
misorientation, respectively. The increase in the intra-layer misorientation is associated with the
dashed line (L)ofare
formation presented
a (sub) in Figure
grain structure. On3.the
The
otherresults
hand,showed large variation
low misorientation regionsacross
in thisthe individual
profile are
layer,associated
where average values of 4.06 ◦ and 6.77◦ were recorded for point-to-origin and point-to-point
with the formation of dislocation-cell structure. Based on the EBSD measurements of the
misorientation,
DSR-deformed respectively.
sample, it isTheworth increase
pointinginout the intra-layer
that misorientation
the traditional is associated
definition of the grain size iswith
not the
formation
enough of here,
a (sub) grain
where substructure.
structuresOn theclear
with otherorientation
hand, lowgradients
misorientation
are formedregions
afterinthethis
DSRprofile
are associated with the formation of dislocation-cell structure. Based on the EBSD measurements of
the DSR-deformed sample, it is worth pointing out that the traditional definition of the grain size
Metals 2017, 7, 494 4 of 10

is not enough here, where sub structures with clear orientation gradients are formed after the DSR
Metals 2017, 7, 494 4 of 10
deformation.
Metals 2017, Due
7, 494 to these gradients, two (non-neighboring) points belonging to the same 4grain of 10 can
be highly misoriented.
deformation. Due toConsequently,
these gradients,the twocalculation of grain
(non-neighboring) size may
points characterize
belonging to the same both grains
grain can and
deformation.
subgrains.
be highly Due to these
Themisoriented.
distribution ofgradients,
the (sub)two
Consequently, the (non-neighboring)
grain size of the
calculation 6061points
of grain belonging
Al alloy
size may deformed to theby
characterize same
both grain
thegrains
DSRandcan
process
be
(Figure highly
subgrains.
4a) misoriented.
shows Thethat Consequently,
distribution
a significant of thefraction
(sub) the calculation
grain
(~19%)size of of grain
of grains
the sizealloy
6061have
Al maydeformed
characterize
diameters both0.1
lessbythan
the grains
DSR and
process
µm, whereas
subgrains.
the average 4a)The
(Figure diameters
showsdistribution
that
(dave of the
a significant
) lies (sub)
withinfractiongrain size
(~19%)
0.4–0.5 µm. of the
ofIn 6061
grains Al alloy
have
addition, deformed
diameters
~40% ofless by the
thethan
grain DSR processhave
0.1boundaries
µm, whereas
(Figure 4a) shows
the average that a(d
diameters significant fraction
ave) lies within
◦ (~19%)
0.4–0.5 µm.of In
grains have diameters
addition, ~40% of the lessgrain
thanboundaries
0.1 µm, whereas have
misorientation angles higher than 15 (high-angle grain boundaries (HAGBs)), as shown by Figure 4b.
the average diameters
misorientation (dave) lies
angles higher thanwithin 0.4–0.5 µm.grain
15° (high-angle In addition,
boundaries~40%(HAGBs)),
of the grain boundaries
as shown have
by Figure
The precipitation behavior of 6061 Al alloy subjected to DSR deformation was investigated
misorientation
4b. angles higher than 15° (high-angle grain boundaries (HAGBs)), as shown by Figure
by Kim4b. etThe
al. precipitation
[11]. Theybehavior found ofthat the features of precipitates after the DSR deformation,
6061 Al alloy subjected to DSR deformation was investigated by
including
Kim The number,
et al. size,
precipitation
[11]. They foundshape
behavior and
thatofthe distribution,
6061 Al alloy
features are mainly
of subjected
precipitatesto DSR related
after to the
deformation
the DSR initial
was microstructure
investigated
deformation, includingby
(before
Kimdeformation).
et al.size,
number, Their
[11]. shape
They results
found
and thatrevealed
the features
distribution, thatmainly
are ofthe sample
precipitates
related with
to a
after fully-annealed
the
the DSR deformation,
initial structure
microstructure possessed
including
(before
a small number
number,
deformation).size,of precipitates
shape
Their and revealed
results after that
distribution, thethe DSR
are deformation.
mainly
sample related
with to Inthethe
a fully-annealed presented
initial work, accordingly,
microstructure
structure possessed (before
a small
deformation).
numberwas
the sample Their results
of precipitates
subjected to revealed
aftera the
heat DSR that the sample
deformation.
treatment at 550 In ◦the
with a fully-annealed
C presented
for work,
3 h followed structure possessed
accordingly,
by air the asample
cooling small
to obtain
number
was of
subjected precipitates
to a heat after the
treatment DSR
at 550deformation.
°C for 3 h In the
followed presented
by air work,
cooling
a fully-annealed structure (Figure 1). In addition, the rolling temperature (RT) employed here is a less to accordingly,
obtain a the sample
fully-annealed
was subjected
structure
than ideal aging to a1).
(Figure heat
temperature treatment
In addition,
of 6061 atAl
the 550alloy
rolling°C temperature
for 3 h followed
(~170 ◦ C). (RT)by air cooling
employed hereto is
obtain
a lessathan
fully-annealed
ideal aging
structure
temperature (Figure 1). In
of 6061 Aladdition,
alloy (~170 the°C).
rolling temperature (RT) employed here is a less than ideal aging
Based on this discussion, it can be noted that the effect of the DSR deformation and pre/post heat
temperature
Based on ofthis
6061 Al alloy (~170
discussion, it can°C).
be noted that the effect of the DSR deformation and pre/post heat
treatment on the precipitation behavior of Al alloys should be investigated in more detail using high
treatment on the precipitation behaviornoted
Based on this discussion, it can be of Althat theshould
alloys effect ofbethe DSR deformation
investigated in moreand pre/post
detail using heat
high
resolution TEM.
treatment on
resolution TEM. the precipitation behavior of Al alloys should be investigated in more detail using high
resolution TEM.

Figure 3. Misorientation profile along the dashed line taken from the rectangle A in the DSR-deformed
Figure 3. Misorientation profile along the dashed line taken from the rectangle A in the DSR-deformed
Figure
6061 Al3.alloy
Misorientation
(Figure 2a).profile along the dashed line taken from the rectangle A in the DSR-deformed
6061 Al alloy (Figure 2a).
6061 Al alloy (Figure 2a).

Figure 4. (a) Grain size distribution and (b) grain boundaries misorientations of the DSR-deformed
Figure
6061 Al4.alloy.
(a) Grain size distribution
The green and
line in Figure 4a(b) grain
shows boundariesthe
additionally misorientations of the DSR-deformed
grain size distribution.
Figure 4. (a) Grain size distribution and (b) grain boundaries misorientations of the DSR-deformed
6061 Al alloy. The green line in Figure 4a shows additionally the grain size distribution.
6061 Al alloy. The green line in Figure 4a shows additionally the grain size distribution.
Metals 2017,7,7,494
Metals2017, 494 5 5ofof1010

3.2. As-Annealed Samples

3.2. As-Annealed Samples
3.2.1. Microhardness
3.2.1. Microhardness
Figure 5a shows microhardness of the DSR-deformed 6061 Al alloy samples as a function of the
Figure 5a shows microhardness of the DSR-deformed 6061 Al alloy samples as a function of
annealing temperature. The curve obtained in Figure 5a exhibited the following three different
the annealing temperature. The curve obtained in Figure 5a exhibited the following three different
regions (i) the microhardness decreases slightly until ~225 °C. This range corresponds to the recovery
regions (i) the microhardness decreases slightly until ~225 ◦ C. This range corresponds to the recovery
in the materials. (ii) The microhardness decreases sharply, i.e., at a steeper slope on the curve, from
in the materials. (ii) The microhardness decreases sharply, i.e., at a steeper slope on the curve,
225 to 350 °C and (iii) the curve levels off at temperatures higher than 350 °C. The sharp decrease of
from 225 to 350 ◦ C and (iii) the curve levels off at temperatures higher than 350 ◦ C. The sharp decrease
the microhardness in the second region of the curve suggests the occurrence of material softening
of the microhardness in the second region of the curve suggests the occurrence of material softening
induced by recrystallization [20]. To show the effect of the annealing temperature on the softening
induced by recrystallization [20]. To show the effect of the annealing temperature on the softening
behavior of the DSR-deformed 6061 Al alloy, the softened fraction (X) was calculated as follows
behavior of the DSR-deformed 6061 Al alloy, the softened fraction (X) was calculated as follows [21,22]:
[21,22]:
Hd −−HHtt
== H
XX d (1)
Hd − H0 (1)
Hd − H0
where Hd , Ht and H0 are the microhardness after DSR deformation, the instantaneous microhardness
where Hd, Ht and H0 are the microhardness after DSR deformation, the instantaneous microhardness
at any temperature, and the microhardness of the initial sample prior to DSR, respectively. Figure 5b
at any temperature, and the microhardness of the initial sample prior to DSR, respectively. Figure 5b
shows the softened fraction at the various annealing temperatures used in this work. After annealing
shows the softened fraction at the various annealing temperatures used in this work. After annealing
at 225 ◦ C for 1 h, the estimated softened fraction of the annealed sample showed a ~2.99% reduction
at 225 °C for 1 h, the estimated softened fraction of the annealed sample showed a ~2.99% reduction
compared to the DSR-deformed sample. The softened fraction of the sample increased significantly
compared to the DSR-deformed sample. The softened fraction of the sample increased significantly
after annealing at temperatures between 225 and 350 ◦ C, where the samples annealed at 275, 325 and
after annealing at temperatures between 225 and 350 °C, where the samples annealed at 275, 325 and
350 ◦ C showed ~45%, ~79.8% and ~99.8% softened fraction compared to the as-deformed sample.
350 °C showed ~45%, ~79.8% and ~99.8% softened fraction compared to the as-deformed sample.

Figure5.5.Effect
Figure Effectofofthe
theannealing
annealingtemperature
temperatureon on(a)
(a)microhardness
microhardnessand
and(b)
(b)softened
softenedfraction
fractionofofthe
the
DSR-deformed 6061 Al alloy. The different color remarks along the dashed line in this figure
DSR-deformed 6061 Al alloy. The different color remarks along the dashed line in this figure indicate indicate
theannealed
the annealedsamples
samplesused
usedtotoinvestigate
investigatethe
themicrostructural
microstructuralevolution
evolutionduring
duringannealing.
annealing.

3.2.2. Microstructure
3.2.2. Microstructure
The microstructural evolution of the samples annealed at 225 °C, 275 °C, 325 °C and 350 °C,
The microstructural evolution of the samples annealed at 225 ◦ C, 275 ◦ C, 325 ◦ C and 350 ◦ C, which
which belong to the second region (ii) as indicated by the colored symbols in Figure 5a, were
belong to the second region (ii) as indicated by the colored symbols in Figure 5a, were investigated to
investigated to understand the softening behavior of the DSR-deformed 6061 Al alloy plates during
understand the softening behavior of the DSR-deformed 6061 Al alloy plates during the heat treatment.
the heat treatment. The EBSD maps (grain boundaries maps) in Figure 6 showed that the lamellar
The EBSD maps (grain boundaries maps) in Figure 6 showed that the lamellar structure was gradually
structure was gradually broken-down to form the equiaxed grains. On the other hand, at 275 °C,
broken-down to form the equiaxed grains. On the other hand, at 275 ◦ C, some areas showed the
some areas showed the lamellar structure obtained by the initial DSR deformation, as indicated by
lamellar structure obtained by the initial DSR deformation, as indicated by the dashed rectangles in
the dashed rectangles in Figure 6b. This was shown further by partitioning of the recrystallized grains
Figure 6b. This was shown further by partitioning of the recrystallized grains of the samples treated at
of the samples treated at 225, 275, 325 and 350 °C using the criteria of GOS [19] (Figure 6e–h). The
225, 275, 325 and 350 ◦ C using the criteria of GOS [19] (Figure 6e–h). The most obvious and expected
most obvious and expected observation from Figure 6e–h is that the fraction of the recrystallized
observation from Figure 6e–h is that the fraction of the recrystallized grains increased with increasing
grains increased with increasing the temperature, where recrystallizations corresponding to ~18%,
Metals 2017, 7, 494 6 of 10

Metals 2017, 7, 494 6 of 10

the temperature, where recrystallizations corresponding to ~18%, ~31%, 52% and ~84% were measured
◦
after the heat treatment at 225, 275, 325 and 350 C, respectively. In addition, the larger fraction
~31%, 52% and ~84% were measured after the heat treatment at 225, 275, 325 and 350 °C, respectively.
of recrystallized microstructures of the sample annealed at 350 ◦ C (Figure 6h) resulted in the low
In addition, the larger fraction of recrystallized microstructures of the sample annealed at 350 °C
microhardness values, as shown in Figure 5a.
(Figure 6h) resulted in the low microhardness values, as shown in Figure 5a.

Figure 6. Grain boundaries maps and recrystallized microstructures of the DSR-deformed 6061 Al
Figure 6. Grain boundaries maps and recrystallized microstructures of the DSR-deformed 6061 Al alloy
alloy annealed for 1 h at (a,e) 225 °C (b,f) 275 °C (c,g) 325 °C (d,h) 350 °C.
annealed for 1 h at (a,e) 225 ◦ C (b,f) 275 ◦ C (c,g) 325 ◦ C (d,h) 350 ◦ C.
Figure 7 presents the microstructural parameters of the annealed plates, including the grain size,
grain shape7aspect
Figure presents theand
ratio microstructural
grain boundary parameters of the annealed
misorientations. The grain plates,
size including
distributionsthe of
grain
the
size, grainplates
annealed shapeshown
aspectinratio and7bgrain
Figure clearlyboundary
show that misorientations.
after annealing The at 225grain
°C andsize275
distributions of
°C for 1 h, the
the annealed plates shown in Figure 7b clearly show that after annealing at 225 ◦ C and 275 ◦ C for
grain size increased from ~0.9 µm, which are still submicron grains, to ~2.2 µm (Figure 7b,d). After
1annealing
h, the grain
at size
325 increased
°C and 350 from°C,~0.9 µm, whichchange
a significant are stillinsubmicron grains, to ~2.2
grain morphology was µm (Figurewhere
observed, 7b,d).
After annealing ◦ ◦
equaixed grainsatwith
325 shape
C andaspect
350 C, a significant
ratios of 0.6 andchange in grain
0.62 were morphology
obtained was observed,
after annealing at 325 °Cwhere
and
equaixed grains with shape aspect ratios of 0.6 and 0.62 were obtained after annealing at 325 ◦C
350 °C, respectively (Figure 7a,d). The distributions of the grain boundary misorientations in Figure
and 350 ◦ C, respectively
7c revealed (Figure
that the fraction 7a,d). The
of HAGBs distributions
evolved during the of the
heatgrain boundary
treatment misorientations
of the deformed plates in
Figure 7c revealed
increased that the fraction
with increasing of HAGBs where
the temperature, evolved~44%,during the heat
~60%, ~68% treatment
and ~77% of the
of deformed
the grain
plates increased
boundaries in thewith increasing
samples annealedthe temperature,
at 225 °C, 275 where
°C, 325~44%,
°C, and~60%,
350 °C~68%for 1and ~77% of the grain
h, respectively, had a
boundaries inmisorientation
the samples annealed at 225 ◦ ◦
C, 275 atC, 325 ◦ ◦
high angle of (>15°). After annealing 225 °C,C,theand 350 C forgenerated
dislocations 1 h, respectively, had
by the plastic
adeformation
high angle of misorientation (>15 ◦ ). After annealing at 225 ◦ C, the dislocations generated by the
(DSR) were absorbed at the boundaries. At the same time, this absorption led to an
plastic
increasedeformation (DSR) wereAfter
in the misorientation. absorbed at the at
annealing boundaries. At the same
275 °C, however, sometime,
LAGBs thisare
absorption led to
still observable
an increase in the misorientation. After annealing ◦
at 275 toC,the
however, some LAGBs are stillInobservable
within the deformed grains, which might be attributed non-absorbed dislocations. addition,
the fraction of LAGBs observed in the samples after annealing at 325 °C and 350 °C led to the
evolution of coarse grains surrounded by HAGBs, as shown by the arrows in Figure 6c,d.
Metals 2017, 7, 494 7 of 10

within the deformed grains, which might be attributed to the non-absorbed dislocations. In addition,
the fraction of LAGBs observed in the samples after annealing at 325 ◦ C and 350 ◦ C led to the evolution
of coarse grains surrounded by HAGBs, as shown by the arrows in Figure 6c,d.
Metals 2017, 7, 494 7 of 10

Figure 7. (a) Grain shape aspect ratio, (b) grain size, (c) grain boundaries misorientation and (d)
Figure 7. (a) Grain shape aspect ratio, (b) grain size, (c) grain boundaries misorientation and (d) average
average aspect ratio and grain size values of the DSR-deformed 6061 Al alloy annealed at different
aspect ratio and grain size values of the DSR-deformed 6061 Al alloy annealed at different temperatures for
temperatures for 1 h. The columns used in Figure 7d are corresponding to the investigated samples
1 h. The columns used in Figure 7d are corresponding to the investigated samples remarked in Figure 5a.
remarked in Figure 5a.

After ◦
After annealing
annealingatat225 225C,°C,local imbalances
local imbalances in surface tension
in surface resulting
tension from the
resulting fromtransverse LAGBs
the transverse
can lead to pinch-off of the lamellar HAGBs formed after DSR deformation
LAGBs can lead to pinch-off of the lamellar HAGBs formed after DSR deformation and subdivision and subdivision of the
elongated grains into shorter segments (Figure 8a). Examples of this
of the elongated grains into shorter segments (Figure 8a). Examples of this behavior can be seen behavior can be seen clearly in
the highinmagnification
clearly TEM images
the high magnification TEMpresented in Figurein8b.
images presented In addition,
Figure the verythe
8b. In addition, fine
verynew grains
fine new
(<100 nm, indicated by the arrows in Figure 8c) observed near the grain
grains (<100 nm, indicated by the arrows in Figure 8c) observed near the grain boundaries confirmed boundaries confirmed that
the ◦
thatrecrystallization
the recrystallization was activated
was activated after 225
after C.
225 The°C.recrystallized grainsgrains
The recrystallized typically grow from
typically grownuclei
from
formed by recovery within the rolling components [23]. Generally,
nuclei formed by recovery within the rolling components [23]. Generally, the microstructure the microstructure evolution during
annealing of Al alloys
evolution during subjected
annealing of Altoalloys
ARB subjected
deformation to ARBis characterized
deformationby nucleation andbygrowth
is characterized [24].
nucleation
However,
and growth the[24].
present resultsthe
However, showed
present a different trend, in
results showed which the
a different lamellar
trend, HAGBs
in which the pinching-off
lamellar HAGBs and
nucleation followed by growth co-exist. This, in turn, is attributed to processing
pinching-off and nucleation followed by growth co-exist. This, in turn, is attributed to processing characteristics of these
methods. In ARB,
characteristics the sample
of these methods.is subjected
In ARB,tothe a high
sample amount of strain,towhich
is subjected a highenhances
amountthe recovery
of strain, rate
which
and increases
enhances the the fraction
recovery of HAGBs
rate as a result.
and increases However,
the fraction of in the DSR
HAGBs asprocess,
a result.the quick dissipation
However, in the DSR of
deformation and friction heats from a thin sheet with a high surface/volume
process, the quick dissipation of deformation and friction heats from a thin sheet with a high ratio to the cold rolls
lead to reductionratio
surface/volume of recovery
to the cold rate. Additionally,
rolls lead to reductionthe fraction of HAGBs
of recovery achieved by the
rate. Additionally, theDSR is still
fraction of
larger than those achieved by conventional methods (symmetric cold
HAGBs achieved by the DSR is still larger than those achieved by conventional methods (symmetric rolling) [9]. In accordance with
the
coldprevious
rolling) ideas,
[9]. In the mechanism
accordance withthattheisprevious
responsible ideas,forthe
themechanism
structure evolution during annealing
that is responsible for the
of the DSRed 6061 Al alloy samples is related to the medium fraction
structure evolution during annealing of the DSRed 6061 Al alloy samples is related to the medium of HAGBs. At this fraction,
the HAGBs
fraction pinching-off
of HAGBs. to divide
At this fraction,the the
lamellar
HAGBs structure and nucleation
pinching-off to divide at the
the lamellar
highly-deformed
structureareasand
simultaneously occur.
nucleation at the highly-deformed areas simultaneously occur.
Metals 2017, 7, 494 8 of 10

Metals 2017, 7, 494 8 of 10

Figure 8. TEM (Transmission Electron Microscopy) images of the DSR-deformed 6061 Al alloy plates
Figure 8. TEM (Transmission Electron Microscopy) images of the DSR-deformed 6061 Al alloy plates
annealed at 225 °C for 1 h: (a) general microstructure; (b) pinching-off of the lamellar HAGBs (high-
annealed at 225 ◦ C for 1 h: (a) general microstructure; (b) pinching-off of the lamellar HAGBs
angle grain boundaries) formed after DSR deformation and subdivision of the elongated grains into
(high-angle grain boundaries) formed after DSR deformation and subdivision of the elongated grains
shorter segments; (c) evolution of fine recrystallized grains.
into shorter segments; (c) evolution of fine recrystallized grains.

In general, the EBSD maps and microstructural parameters of the 6061 Al alloy samples during
In general,
annealing the EBSD
at different maps and microstructural
temperatures for 1 h showed parameters of the 6061 Al
that the microstructure alloy samples
evolves during
in a continuous
annealing
manner, inatthat
different temperatures
no local for 1front
transformation h showed
can bethat the microstructure
observed. This behaviorevolves
was alsoin a reported
continuous by
manner,
the present authors, in which the texture evolution during the annealing treatment of theby
in that no local transformation front can be observed. This behavior was also reported the
DSR-
present
deformed authors,
6061 Alin alloy
whichsamples
the texture
was evolution during
investigated [25].the
Theannealing treatment
results showed thatofthe
themanner
DSR-deformed
in which
6061 Al alloy samples was investigated [25]. The results showed that the manner
the various components of rolling, shear and recrystallization textures changed, was relatedin which the various
to the
components of rolling, shear and recrystallization
operation of continuous recrystallization. textures changed, was related to the operation of
continuous recrystallization.
The results presented in this work mostly involve the grain structure evolution, but the
The results presented
precipitation behavior uponin this work
annealing mostly
of the involve thesamples,
DSR-deformed grain structure
which is evolution,
also one of but the
the key
precipitation behavior upon annealing of the DSR-deformed samples, which is also
aspects of the microstructure for 6xxx series Al alloys, has not been discussed. Accordingly, future one of the
key aspects of
experiments thebemicrostructure
will for 6xxx
designed to address thisseries
point.Al alloys, has not been discussed. Accordingly,
future experiments will be designed to address this point.
4. Conclusions
4. Conclusions
Ultrafine grained 6061 Al alloy plates (0.9 wt % Mg) manufactured by room-temperature DSR
Ultrafine grained 6061 Al alloy plates (0.9 wt % Mg) manufactured by room-temperature DSR
deformation were annealed isochronally at temperatures between 150 and 400 ◦°C for 1 h. The basic
deformation were annealed isochronally at temperatures between 150 and 400 C for 1 h. The basic
results and conclusions from the present investigation are as follows:
results and conclusions from the present investigation are as follows:
1. The DSR-deformed 6061 Al alloy showed a lamellar boundary structure composed mostly of
1. The DSR-deformed
subgrains with high 6061 Al alloy
fraction showed a lamellar boundary structure composed mostly of
of LAGBs.
subgrains
2. The withofhigh
hardness the fraction of LAGBs.
DSRed plates slightly decreased with increasing temperature until 225 °C
2. The hardness of the DSRed plates slightly decreased with
and decreased sharply after annealing at temperatures increasing
higher than 225temperature
°C. until 225 ◦ C
and decreased sharply ◦
3. The microstructure of after
the annealing at temperatures
DSR-fabricated higher thanfrom
plates transformed 225 the
C. lamellar boundary
3. structure into a coarse-grained
The microstructure structure during
of the DSR-fabricated annealing and
plates transformed thethe
from extremely
lamellar fine grainsstructure
boundary detected
in
intothe sample annealed
a coarse-grained at 225during
structure °C suggested
annealingthat
andthe
the recrystallization became
extremely fine grains activeinafter
detected the
annealing at 225 ◦ C suggested
at this temperature
sample annealed (225 °C).that the recrystallization became active after annealing at
this temperature (225 ◦ C).
Metals 2017, 7, 494 9 of 10

Acknowledgments: This research was supported by National Research Foundation (NRF) of Korea (2017R1C1B5017204).
Author Contributions: Young Gun Ko conceived and designed the experiments; Kotiba Hamad performed the
experiments; analyzed the data; and wrote the paper. Both authors discussed the results.
Conflicts of Interest: The authors declare no conflict of interest.

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