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Copyright © 2017 American Scientific Publishers
Nanoscience and Nanotechnology
All rights reserved Vol. 17, 4153–4156, 2017
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Variation of Precipitation Behavior with Heat

Treatment of Friction Stir Processed AA6082
JaeHwang Kim1 , Ram Song2 , and KwangJin Lee1 ∗
1
Carbon and Light Material Application Group, Korea Institute of Industrial Technology, 100, Jipyungsun Sandan 3gil,
Backsan-Myeon, Gimje-si, 54325, South Korea
2
Department of Metallurgy and Ceramics Science, Tokyo Institute of Technology, 2-12-1, O-Okayama, Meguro-ku, Tokyo, 152-8552, Japan

The extruded AA6082 was heat treated after friction stir processing (FSP) in this study. The grain
size is affected by the friction heat during FSP. Smaller grain size is confirmed in the stir zone (SZ)
than any other regions due to the dynamic recrystallization. Hardness is substantially enhanced
during heat treatment after FSP. Hardness is highly fluctuated in the region of heat affected zone
(HAZ) during aging process. The region of HAZ is divided into three regions called as HAZ1, HAZ2
and HAZ3 where the area of HAZ1, HAZ2 and HAZ3 is defined as the area close to SZ, middle of
HAZ and close to base material (BM), respectively. The crystal structure of nano size precipitates
is revealed using high resolution transmission electron microscope. The maximum hardness is
obtained in base material region due to the formation of the  phase with high number density.
On the other hand, the minimum hardness is identified in HAZ2 since the grain is grown and the 
phase is formed duringIP:FSP.
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1. INTRODUCTION 2. EXPERIMENTAL DETAILS

The AA6082 has been widely used for the vehicles as a
typical heat-treatable alloy with the high specific strength
due to its good age-hardening response. The most accepted
precipitation sequence in Al–Mg–Si alloys is SSSS → GP
zone →  →  rods + lath + plate-like particles → 
where, SSSS is supersaturated solid solution.1 2 Under-
standing for the early stage of age-hardening3 4 becomes
attractive in order to control microstructure5 6 and mechan-
ical properties7 8 in Al–Mg–Si alloys.
The grain refinement leading strength improvement
based on the Hall-Petch relation9 10 can be achieved
through the severe plastic deformation (SPD) process.11
Friction stir processing (FSP) is one of the SPD processes
and it causes intense plastic deformation. The frictional
heat is generated during FSP where the temperature of
the material is rapidly increased. In order to obtain high
strength Al alloys, combination of grain refinement and
precipitate formation is required through FSP and aging
processes. However, the age-hardening behavior for the
FSPed alloys has not been clearly revealed in Al–Mg–Si
alloys yet. Therefore, the age-hardening behavior of FSPed
AA6082 is investigated in this study.
∗
Author to whom correspondence should be addressed.
AA6082 is manufactured by porthole extrusion method
with the thickness of 6 mm. The chemical composition of
the material used in this study is summarized in Table I.
The extruded AA6082 was subjected to solution treat-
ment at 530  C for 3.6 ks and then immediately water
quenched for 60 sec. The FSP was conducted at con-
stant tool rotation speed and traveling speed with 1000
rpm and 333 mm/min, respectively. The cylindrical FSP
tool was made of SKD-61. The diameter of shoulder and
probe was 15 and 6 mm, respectively. The artificial aging
was conducted at 190  C for 14.4 ks for understanding
the formation behavior of the precipitates. Micro Vickers
hardness measurement was employed in the mid-thickness
region across the cross-section under a load of 100 g
for 10 s. Microstructural observation was performed using
field emission scanning electron microscope (FE-SEM)
with electron back scatter diffraction (EBSD), transmission
electron microscope (TEM) and high resolution transmis-
sion electron microscope (HRTEM) with 100 kV.
3. RESULTS AND DISCUSSION
Figure 1 shows overview of cross-section for the FSPed
AA6082. A defect-free specimen was obtained as shown

J. Nanosci. Nanotechnol. 2017, Vol. 17, No. 6 1533-4880/2017/17/4153/004 doi:10.1166/jnn.2017.13415 4153

Variation of Precipitation Behavior with Heat Treatment of Friction Stir Processed AA6082 Kim et al.

Table I. Chemical composition of the material used in this research 140

(mass %). FSP+T6
130 BM FSP
Si Mg Fe Mn Fe Others Al SZ
120
0.65 0.66 0.16 0.75 0.16 ≤0.2 Bal.

Hardness, Hv
110 HAZ3
HAZ1
100
in Figure 1(a). The enlarged area for the dashed blue HAZ2
90
line in Figure 1(a) is shown in Figure 1(b). A, B and C
regions in this study are called as stir zone (SZ), heat 80
affected zone (HAZ) and base material (BM), respectively. 70
Basically, higher friction heat is generated in the order of
60
SZ, HAZ and BM during FSP.
Figure 2 shows the hardness for FSPed region with and 0 5 10 15 20
Distance from the center, mm
without heat treatment to understand the effects of heat
treatment on the age-hardening behavior. The hardness is Figure 2. Hardness profile of the FSPed AA6082 extrusion in mid-
clearly increased during aging treatment due to the for- thickness.
mation of precipitates. The hardness changes are more
clearly identified in the heat treated samples than that of the marked area with the black color is excluded for the
the FSPed one as shown in Figure 2. The hardness was measurement of the grain size as shown in Figure 3(b).
continuously measured from the SZ to the BM region. Figure 4 shows the hardness and average grain size with
The hardness is gradually decreased from the SZ to HAZ. the different regions of FSP followed by the heat treat-
The minimum hardness is confirmed at the HAZ. On the ment in the AA6082. The grain size is gradually increased
other hand, the hardness is gradually increased from HAZ from SZ to BM. The grain size is smaller in SZ due to the
to BM. The recrystallization and age-hardening behavior dynamic recrystallization than any other regions of FSP.
are simultaneously considered to understand the relation On the other hand, hardness is decreased from the SZ
between the microstructure and mechanical properties in to HAZ and increased from HAZ to BM as revealed in
this study. In order to understand the effects of grain size Figure 4. In order to understand the reason of the hardness
on the hardness, hardness test IP: is 89.191.226.248
firstly performed On:
and Mon, 15 Junwith
changes 2020
the09:03:00
region of FSP, the area of HAZ is divided
Copyright: American
the grain size was analyzed using EBSD. Figure 3 shows Scientific Publishers
into HAZ1,
Delivered by Ingenta HAZ2 and HAZ3. The area of HAZ1, HAZ2
the method of the grain size measurement. The area was and HAZ3 is defined as the area close to SZ, middle of
selected after checking the hardness value as shown in
Figure 3(a). Surrounding of the hardness indentation is
selected as the measured area for the grain size. Namely, (a) (b)

(a)

2 mm

(b)

70 um 70 um
C
200 um
Figure 3. Example of grain size measurement using FE-SEM EBSD.
(a) selected area of FSPed AA6082 followed by the heat treatment with
Figure 1. (a) Cross-section of friction-stir-processed AA6082 extrusion different hardness (b) measured area for the average grain size except
(b) dashed area of (a). A, B and C region is distinguished as stir zone, the area of hardness measurement. Grain size does hardly change during
heat affected zone and base material. aging process.

4154 J. Nanosci. Nanotechnol. 17, 4153–4156, 2017

Kim et al. Variation of Precipitation Behavior with Heat Treatment of Friction Stir Processed AA6082

20 130 (a) (b)

18 120
Grain size, µm

16 110 75

Hardness, Hv

[010]Al
14 100

12 90 [100]Al

10 80 5 nm
Grain size
Hardness (c) (d)
8 70
SZ HAZ1 HAZ2 HAZ3 BM

Figure 4. Hardness and average grain size with different regions of FSP
followed by heat treatment in the AA6082.

HAZ and close to BM, respectively. A similar hardness is

identified in the HAZ1 and HAZ3. The minimum hardness
is confirmed in HAZ2. 5 nm
Figure 5 shows the TEM and HRTEM images for the (e) (f)
FSPed AA6082 after aging at 190  C for 14.4 ks with
the different regions. All the micrographs are obtained
on 001 zone axis. The diffraction patters are obtained
and shown at the right bottom side of the TEM micro- 60
graphs. Precipitates with the different regions are investi-
gated since the hardness is substantially increased during
aging process. In the case of HAZ region, two different
IP: 89.191.226.248 On: Mon, 15 Jun 2020 09:03:00
regions such as HAZ1 and HAZ2 areCopyright:
selected due to the Scientific Publishers
American 5 nm
difference of the hardness as identified in FiguresDelivered
2 and 4. by Ingenta
(g) (h)
HRTEM images are obtained for distinguishing the crys-
tal structure of the precipitates. Marioara et al.2 revealed
that the  phase having the monoclinic angle is simply
determined through observation of the cross-sections. The
structure of precipitates is also determined by the mea-
surement of two types of angle and lattice parameter.1 The
lattice parameter of the  phase is 0.67 and 0.77 nm and
the interior angle of the parallelogram network inside pre-
cipitates is 75 .1 In the case of  phase, the interior angle 5 nm
 13
of the parallelogram network inside precipitates is 60 .
Figure 5. TEM and HRTEM micrographs of FSPed AA6082 after
The  phase is formed regardless of the FSPed region as aging at 190  C for 14.4 ks in the SZ (a) and (b), HAZ1 (c) and (d),
shown in Figure 5. Higher number density of the  phase HAZ2 (e) and (f), and BM (g) and (h). All micrographs are taken at
in BM is confirmed than that of SZ. However, the  phase (001) plane.
is formed only in the region of HAZ2. The present authors
noting that the age-hardening behavior is strongly affected
believe that the  phase is formed during FSP, resulting
by friction heat during FSP.
in that the hardness in the area of HAZ2 is lower than any
other region of FSP. It causes that amount of solute atoms
such as Mg and Si is insufficient to form the  phase 4. CONCLUSION
during aging process since  phase is formed before heat The precipitation behavior of FSPed AA6082 was inves-
treatment. It is noted that maximum hardness is obtained tigated using hardness and grain size measurements and
in BM due to the formation of the  phase with high observation of precipitates. The obtained results are sum-
number density. On the other hand, the minimum hardness marized as follows.
is identified in HAZ2 since the grain is grown and the  (1) Friction stir processing of AA6082 extrusion was suc-
phase is formed during FSP. Different number density and cessfully carried out without apparent defects. The Smaller
the precipitates are revealed with the region of FSP since grain size is identified in the SZ than any other regions
the friction heat is differently generated. It is importantly due to the dynamic recrystallization during FSP.

J. Nanosci. Nanotechnol. 17, 4153–4156, 2017 4155

Variation of Precipitation Behavior with Heat Treatment of Friction Stir Processed AA6082 Kim et al.

(2) Hardness is substantially increased during aging pro-
cess due to the formation of nano size precipitates. The
 phase is formed regardless of the FSPed regions. High
number density of the  phase in BM is revealed, result-
ing in enhancement of hardness. On the other hand, the
minimum hardness is confirmed in HAZ2 (middle of HAZ
area) since the grain is grown and the  phase is formed
during FSP.
Acknowledgments: This work was supported by Korea
Institute of Industrial Technology.
References and Notes
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Received: 1 December 2015. Accepted: 30 April 2016.

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