Science and Technology of Welding and Joining

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Microstructure and microhardness of aluminium

alloy friction stir welds with heat treatment

Y. X. Huang, L. Wan, Z. L. Lv, S. X. Lv, L. Zhou & J. C. Feng

To cite this article: Y. X. Huang, L. Wan, Z. L. Lv, S. X. Lv, L. Zhou & J. C. Feng (2016):
Microstructure and microhardness of aluminium alloy friction stir welds with heat treatment,
Science and Technology of Welding and Joining, DOI: 10.1080/13621718.2016.1152748

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Published online: 18 May 2016.

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 Microstructure and microhardness of
aluminium alloy friction stir welds with heat
treatment
Y. X. Huang∗ 1, L. Wan1, Z. L. Lv1, S. X. Lv1, L. Zhou2 and J. C. Feng1,2
In this study, the Al–Mg–Si aluminium alloy with a T6 temper is self-support friction stir welded, and
the effect of post-weld heat treatment on joints is investigated by detailed microstructural
investigations and microhardness measurements. The hardness decreases from average 59 to
52 HV with holding time ranging from 10 to 60 minutes at temperature 723 K. With increasing
holding temperature, the microhardness becomes more uniform and increases. Microhardness
Downloaded by [University of Nebraska, Lincoln] at 01:41 26 May 2016

profiles are explained by precipitate distributions and precipitation sequences. The fine grain
structure undergoes abnormal grain growth, and the degree of which depends on holding
temperature and intense plastic deformation, and the biggest size is more than 1 mm.
Keywords: Self-support friction stir welding, Post-weld heat treatment, Microstructure, Microhardness, Abnormal grain growth

Introduction İpekoğ lu et al. revealed that FSW resulted in a strength

Al–Mg–Si aluminium alloy is an age-hardened alloy pos-
sessing enhanced strength and extensively employed in
marine frames, pipelines, storage tanks and aircraft appli-
cations.1 The precipitation behaviour of Al–Mg–Si alloys
is generally reported to be: supersaturated solid solution
(SSS) → cluster → GP zones → b′′ → b′ → β.2 Their mech-
anical properties are strongly depended on metastable
precursors of equilibrium β (Mg2Si) phases. Although
the material remains in a solid state during friction stir
welding (FSW), it is subjected to intense plastic defor-
mation at elevated temperatures,3–6 leading to significant
modification of the microstructure and mechanical prop-
erties,7 and the softening problem can be a non-acceptable
problem,8 particularly in age-hardened grades.9,10 The
degree of joint strength loss taking place in weld region
of age-hardened Al alloys depends on weld parameters,
and it takes place even though optimum weld parameters
are used.11 Due to the heat input, although not high
enough to melt the material, it leads to solution and/or
coarsening of strengthening particles in welding nugget
zone (WNZ), and thermo-mechanically affected zone
(TMAZ) and to overage (coarsening of strengthening par-
ticles) in heat-affected zone (HAZ).12 During FSW pro-
cess, frictional heat associated with thermal cycle varies
in transverse direction of the weld and causes an altera-
tion in precipitate distribution present in base material
(BM). These changes in the heat and temperature distri-
bution in welding process alter the strength and ductility
of the joints.13
1
State Key Laboratory of Advanced Welding and Joining, Harbin Institute of
Technology, Harbin 150001, China
2
Shandong Provincial Key Laboratory of Special Welding Technology,
Harbin Institute of Technology at Weihai, Weihai 264209, China
∗
Corresponding author, email yxhuang@hit.edu.cn; cn_hyx@163.com
undermatching when the 7075 Al alloy joined in T6 con-
dition.14 Wan et al. points out that the average microhard-
ness in WNZ near TMAZ was the lowest because of an
overaging effect and the coarser second-phase particles.15
So several investigations were carried out to study
the possibility of improving mechanical properties of
FSW joints by applying post-weld heat treatments
(PWHT).5,16,17 Chaitanya et al. studied the effects of
five different PWHTs on 7039 Al alloy FSW joints in
order to understand their effects on microstructure and
mechanical properties.16 Sato and Kokawa reported that
both direct artificial aging and artificial aging following
solutionising led to an increase in the strength of 6063
Al alloy FSWed joints.17 Safarkhanian et al. reported
that the strength in the joint area of 2024-T4 Al alloy
FSWed joints could be increased by a natural aging fol-
lowing solutionising.8 However, there are also contradict-
ing results in literatures on the influence of PHWT on
mechanical properties of FSWed Al alloys. Elangovan
and Balasubramanian studied the effect of different
PWHTs on 6061-T6 Al alloy FSWed joint performance
and observed that a PWHT consisting of solutionising
and quenching followed by artificial aging resulted in a
loss of strength.1 Mahoney et al. reported that a direct
artificial aging without solutionising did not alter the
yield stress, but decreased tensile strength of the FSWed
7075-T651 Al alloy joints.18 Aydin et al. investigated the
effect of several different PWHTs on the strength of the
weld zone of FSWed 2024-T4 Al alloy joints and reported
that natural aging following solutionising resulted in a
decrease in the strength.19
In this study, 6082-T6 alloy joints are produced by self-
support friction stir welding (SSFSW). The effect of
PWHT on microhardness and microstructure evolution
is investigated. The relations between microhardness

© 2016 Institute of Materials, Minerals and Mining

Published by Taylor & Francis on behalf of the Institute
Received 21 December 2015; accepted 7 February 2016
DOI 10.1080/13621718.2016.1152748 Science and Technology of Welding and Joining 2016 1
 Huang et al. Microstructure and microhardness of aluminium alloy friction stir welds with heat treatment
distribution and microstructure evolution in BM and
WNZ in term of the grain size and strengthening particles
are discussed.
Experimental procedure
The Al–Mg–Si aluminium alloy with a T6 temper (6082-
T6) is used as BM. The 5 mm thick plate is cut into
300×100 mm pieces. The chemical compositions and
mechanical properties are listed in Table 1. The SSFSW
tool with interesting tool profiles consisting of double dis-
symmetrical shoulders (the concave upper shoulder and
the convex lower shoulder) and tapered stir pin made of
high speed steel, as shown in Fig. 1. The upper and
lower shoulders have angles of 87.5° and 75° with the
tool centre axis, respectively. The geometries and features
of the SSFSW tool are listed in Table 2. The plates are
fixed on the clamping apparatus without backing bar.
The SSFSW tool is pressed into the plates at the edge
and starts to weld with 10 mm min−1 welding speed.
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The minimum distance to achieve stable process con-
dition is 12 mm (diameter of the upper shoulder). The
SSFSW process is performed using an FSW machine
(FSW-3LM-003) with rotational speed of 900 rev min−1,
tilt angle of 4°, plunge depth of 0.1 mm and welding
speed of 50 mm min−1. And the joints are cut into two
parts, one part for PWHT and the other for as-welded
examinations. For investigation of the thermal stability,
SSFSWed samples are heat treated in an air furnace for
10, 20 and 60 minutes at temperatures of 723 K, and
then quenched in water. The selected samples are also iso-
thermally annealed for up to 60 minutes at temperatures
ranging from 723 to 823 K and subsequently quenched
in water.
Specimens are cut to carry out microstructural and
mechanical characterisation and prepared according to
standard procedures including grinding, polishing and
etching. The specimens are etched with reagent (1 ml
hydrofluoric acid + 1.5 ml hydrochloric acid + 2.5 ml
nitric acid + 95 ml water) to reveal microstructures. The
microstructure and chemical composition of the joints
are analysed using optical microscopy (OM, Olympus-
MPG3) and scanning electron microscope (SEM, HITA-
CHI S-3500N) equipped with an energy dispersive spec-
trometer (EDS). The microhardness testing is conducted
using a Vickers hardness testing machine (HX-1000)
with a test load of 200 g and an indentation time of 10
seconds. Measurements are performed pointwise in differ-
ent zones.
Results and discussion
Microstructure
As shown in Fig. 2, the initial microstructure of BM con-
sisted of large elongated pancake shaped alpha grains
Table 1 Chemical compositions of 6082-T6 aluminium alloy
Chemical compositions/wt-%
Mg Si Mn Fe Cr Zn Cu Ti
1.10 0.80 0.60 0.50 0.25 0.20 0.10 0.10
2 Science and Technology of Welding and Joining 2016
1 Schematic presentation of the self-supporting friction stir
welding tool
indicating that it was heavily rolled. They are about
100–300 μm in length and 30–60 μm in width. A consider-
able amount of coarse dispersions are randomly distribu-
ted. Black large-round particles and white rod-like
particles are inhomogeneously distributed, as shown in
Fig. 2b and c. The black large-round particles contained
Mg and Si, indicating that they are Mg2Si particles,
whereas black rod-like particles contained Al, Si, Mn
and Fe, indicating that they are AlSiMnFe particles as
shown in inset of EDX point analyses. The 6082-T6 alu-
minium alloy is an age hardenable alloy possessing
enhanced strength due to the precipitation of Mg2Si
phase upon solutionising and artificial aging. The sol-
ution treatment is carried out at 883 K for 1 hour, and
then followed by quenching in water and subsequent by
artificial ageing at 453 K for 8 hours. The solidus temp-
erature of this alloy is about 848 K. The microstructure
of the WNZ is illustrated in Fig. 2d–f. The WNZ is sub-
jected to a high level of plastic deformation and frictional
heating. Fine-grained microstructure with slightly corru-
gated boundaries is formed homogeneously in the whole
area, as shown in Fig. 2d. The dynamic recrystallisation
is responsible for production of new fine grains in the
WNZ.20–22 The grains tend to be corrugated when the
density of dislocations entering the grain boundaries
exceeds their absorption capacity or when the process of
lattice dislocation absorption requires long time.23,24
The similar result is also found in the reference.25,26
Wang et al. points out that the WNZ has much small
equiaxed recrystallised grains and average size of recrys-
tallised grains increases from 2.1 to 6.0 μm with increas-
ing rotational speeds.25 The peak temperature, which
locates 10 mm away from the weld centre on the advan-
cing side, increases from 525 to 603 K with the rotational
speed increasing from 400 to 1000 rev min−1. Chen et al.
studies the temperature distribution and control of 6061
aluminium alloy bobbin tool friction stir welded joints
and shows that the region very close to the WNZ experi-
ences temperature nearer to 753 K which forces the sec-
ondary phase particles in the original phase matrix to
dissolve and produces fine grain structure.26
Figure 2e and f show the typical cross-sectional second-
phase particles distribution in the WNZ. Intense plastic
deformation and frictional heating result in generation
of a recrystallised fine-grained microstructure and more
uniform and intensive second-phase particles within stir-
red zone. Some inhomogeneously distributed large and
round Mg2Si particles are also present in the WNZ.
Al SEM investigations also clearly indicated the presence
of homogeneously distributed finer strengthening par-
Bal. ticles, as shown in Fig. 2f. The precipitation of these
 Huang et al.
Table 2 Welding tool geometries and features for SSFSW
Process Tool geometry Tool material Upper shoulder diameter/mm
SSFSW Conical pin with thread Steel
particles can be attributed to heat input during welding
and the natural aging process. Fu et al. also pointed out
that dissolution for the higher peak temperature and re-
precipitation for the lower cooling rate occurs in the
strengthening-phase particles of the WNZ.27
Effect of holding temperature and time
The microstructures of the SSFSWed joints after static
annealing for 10, 20 and 60 minutes at the temperature
of 723 K, are shown in Fig. 3. In the BM, the small pre-
cipitate free zone (PFZ) is evident along grain boundaries.
The fine-grained structure is coarsened during static
annealing at 723 K, resulting in an increase in average
Downloaded by [University of Nebraska, Lincoln] at 01:41 26 May 2016
grain size. Krishnan shows that the WNZ in FSW 6061
aluminium alloy exhibits coarsened grains after solution
treatment at temperatures between 793 and 833 K.28
Numerous strengthening precipitates have densely distrib-
uted inside the grains. The strengthening precipitates have
coarsened severely. The precipitates near grain boundaries
disappear, and the width of PFZ along the grain bound-
aries has increased compared to the BM microstructure,
as shown in Fig. 3a–c. The Mg and Si atoms are in
solid solution, and the formation of PFZ is due to further
solutioning of precipitates. The strengthening precipitates
existed in WNZ and BM both undergo severe coarsening
and partial dissolution with the increasing of annealing
time, as shown in Fig. 3c, d, g and h. During subsequent
cooling stage or PWHT stage the re-precipitating pro-
cesses of strengthening phase particles occurred in the
WNZ. The longer annealing time accelerated the coarsen-
ing processes. For annealing time 10–60 minutes, due to
the increasing of the annealing time a part of strengthen-
ing-phase particles occurred dissolving and the other
occurred coarsening (Fig. 3d and h).
In order to reveal the microstructure evolution behav-
iour with heat treatment, a schematic presentation is
2 Microstructure feature. a Optical photo of BM; b particles in BM; c higher magnification of BM; d microstructure of WNZ; e
second-phase particles in the WNZ; f higher magnification of WNZ
Microstructure and microhardness of aluminium alloy friction stir welds with heat treatment
Lower shoulder diameter/mm Pin length/mm
12 6 4.6
demonstrated in Fig. 4. During the PWHT, the tiny par-
ticles become more and denser. The particles include
those precipitated along grain boundaries and those are
broken up by rotating stir pin. The heat input makes the
tiny, metastable precipitates to be coarsened (Figs. 3f–h
and 4b). The max temperature of 723 K cannot achieve
the dissolution of stable Mg2Si phase particles, but benefit
atomic diffusion. The diffusive flows of Mg and Si atoms
from tiny precipitates and α-Al matrix will strongly con-
tribute to the growth of the grain boundaries (Fig. 4b).
The concentrations of Mg and Si at the interfaces of
grain boundaries and matrix will decrease.
Figure 5 shows the distributions of strengthening pre-
cipitates with different heat treatment conditions. The
joint with holding temperature of 723 K shows a con-
siderable increase in the density of spherical Mg2Si pre-
cipitates, uniformly distribution throughout the matrix
(Fig. 5b and f ). In the WNZ, a preferentially etched
zone is characterised by a significant refinement of the
second-phase particles, as compared to the WNZ micro-
structure with holding temperature of 773 K, which
showed a dispersion of coarse over-aged particles as
shown in Fig. 5c and g, respectively. The time above the
dissolution temperature is insufficient to cause complete
dissolution of the coarser particles. Murr and co-workers
indicate that some of the precipitates are not dissolved
during welding of alloy 6061.29 The strengthening precipi-
tates undergo severe coarsening and partial dissolution as
a result of the high peak temperatures. PWHT resulted in
the precipitation of homogeneously distributed needle-
shaped strengthening particles in WNZ of the joints pro-
duced in T6-temper condition (Fig. 5h). Sato et al.
showed that a post-weld heat treatment on a 6063-T5 fric-
tion stir weld forces the precipitation of strengthening par-
ticles in regions where the Mg and Si are in solid
solution.30 The strengthening precipitates were re-precipi-
tated preferentially along grain boundaries, sub-grain
Science and Technology of Welding and Joining 2016 3
 Huang et al. Microstructure and microhardness of aluminium alloy friction stir welds with heat treatment
Downloaded by [University of Nebraska, Lincoln] at 01:41 26 May 2016
3 Microstructure evolution with heat treatment conditions. a Unaffected BM; b–d BM with holding time of 10, 20 and 60 minutes;
e as-welded WNZ; f–h WNZ with holding time of 10, 20 and 60 minutes
4 Schematic map of microstructure evolution behaviour
with heat treatment. a Unaffected BM; b PFZ and the pre-
cipitation of second particles; c coarsening of strengthen-
ing particles
4 Science and Technology of Welding and Joining 2016
boundaries, and dislocation cores during cooling. The
WNZ exhibits a supersaturated solid solution state with
a high concentration of vacancies, thereby it promote
the diffusion of the solute atoms to form strengthening
particles during the subsequent cooling stage or PWHT
process compared with the BM microstructures, as
shown in Fig. 5d and h.
Interestingly, PWHT resulted in the formation of
abnormal grain growth (AGG) shown in Fig. 6. The
fine-grained structure developed under FSW is stable
during static annealing at temperatures up to 723 K.
However, with increasing in annealing temperature to
773 K, the abnormal grain growth is characterised by
the evolution of very large grains which are millimetre
scale. The maximum size reaches about 1300 μm. The
AGG formation is quite pronounced, occurring mainly
in the shoulder action regions. Chen et al. studies the
temperature distribution and control of 6061 aluminium
alloy bobbin tool FSW joints and shows that the region
very close to the WNZ experiences temperature nearer
to 753 K which forces the secondary phase particles in
the original phase matrix to dissolve.26 Furthermore, the
extent of AGG is higher in the weld zone of the joint pro-
duced with the holding temperature of 823 K. This clearly
indicates that the holding temperature plays an important
role on the degree of AGG.
The difference in the degree of AGG can be explained
by the amount of plastic deformation and the stored
energy. The plastic deformation in the shoulder action
zone is higher, and AGG is more likely to develop. The
upper and lower shoulder regions both experience signifi-
cant frictional heating and plastic flow owing to the
 Huang et al. Microstructure and microhardness of aluminium alloy friction stir welds with heat treatment

5 Distribution of strengthening precipitates with heat treatment conditions. a Unaffected BM; b–d BM with holding temperature
of 723, 773 and 823 K; e as-welded WNZ; f–h WNZ with holding temperature of 723, 773 and 823 K

contact with the shoulder. The energy stored in the destabilised by dissolution of the pinning phase. During
Downloaded by [University of Nebraska, Lincoln] at 01:41 26 May 2016

shoulder region increases due to finer grains. The AGG
formation degree upon subsequent heat treatment is
higher when the stored energy is high.30 Higher amount
of AGG formation after PWHT is probably due to the
evolution of finer grains, as shown in Fig. 6. This is likely
the reason for the AGG formation in a narrow region
endured the shoulder action. It is important to highlight
the fact that AGG could have initiated by dynamic recrys-
tallisation and continued with subsequent heat treatment.
With the observations of grain size and second-phase par-
ticles within the BM and WNZ, and then the subsequent
development of AGG in the shoulder action region, it can
be argued that the grain size and precipitates morphology
are important to the formation of AGG. Once grain size
decreases, the pressure generated by the driving force for
grain growth will exceed the particle pinning pressure,
leading to AGG.31 It is generally accepted that second-
phase particles have an important effect on the occurrence
of AGG.32 Second-phase particles lead to grain boundary
pinning via the Zener mechanism, which halts grain
growth. The microstructure of Zener-pinned grains is
the PWHT with holding temperature above 773 K frag-
mented and segregated second-phase particles go into
solid solution. With fine grain sizes associated with
SSFSW in shoulder action region, the driving force for
grain growth exceeds particle pinning pressure, leading
to AGG, as shown in Fig. 6.
Microhardness
Figure 7 shows the variations of microhardness distri-
bution of joint cross-section. The microhardness distri-
bution profile of as-welded T6 joint exhibits W-shape
and is corresponding to four distinct microstructural
zones. As illustrated, a microhardness decrease (strength
undermatching) is observed in the HAZ, TMAZ and
WNZ.9,33 The microhardness falls dramatically in the
region that is passed over by the shoulder and the lowest
hardness in as-welded joint is observed at HAZ. The
reason for the hardness decrease is due to the fact that
overaging takes place as a result of heat input during
welding. The heat input during SSFSW leads to solution

6 Abnormal grain growth with post weld heat treatment (823 K, 60 minutes). a–c Upper shoulder action region; d–f lower
shoulder action region

Science and Technology of Welding and Joining 2016 5

 Huang et al. Microstructure and microhardness of aluminium alloy friction stir welds with heat treatment
Downloaded by [University of Nebraska, Lincoln] at 01:41 26 May 2016

7 Microhardness distributions with heat treatment conditions. a As-welded; b 723K-10 minutes; c 723K-20 minutes; d 723K-60
minutes; e 773K-60 minutes; f 823K-60 minutes

and/or coarsening of strengthening particles in WNZ and
TMAZ and overage (coarsening of strengthening par-
ticles) in HAZ. The relative microhardness increase in
the WNZ is due to the grain refinement and the presence
of homogenously distributed precipitated particles. The
hardness is determined by the grain size and the volume
percentage of precipitates and dislocation density.
The PWHT resulted in the deterioration of hardness
value in comparison with as-welded joints. The BM in
initial condition T6 showed a hardness value of 100HV,
but in the as-welded joint the lowest hardness was only
57HV in HAZ. The hardness profiles of the precipi-
tation-hardenable Al alloy depend strongly on precipitate
distributions rather than on the grain structure. The soft-
ening was characterised by dissolution or growth of
strengthening needle-shaped precipitates. The hardness
of the joints which are treated at holding temperature of
723 K exhibits significant decrease. The microhardness
decreased from average 59 to 52HV with holding time
ranging from 10 to 60 minutes. The reason is the differ-
ences in the heat treatments applied, namely a longer
holding time, i.e., 60 minutes at 723 K, which led to overa-
ging, than the shorter holding time, i.e., 10 and 20 minutes
at 723 K, as shown in Fig. 3e–h. The precipitates with
holding temperature of 723 K are coarse and appear to
be agglomerated continuously at the grain boundaries.
The joint experiences a decrease in the density of nee-
dle-shaped precipitates. Instead, the average hardness
exhibits a better dependency on the holding temperature.
The solution treatment with holding temperature of 823
K offered the lowest decrease in the hardness and exhib-
ited the highest hardness of 90HV which is near that of
the WNZ for as-welded joint. The PWHT recovered par-
tial hardness loss and their microhardness profiles became
quite homogeneous across the joint area when the holding
temperature ranging from 723 to 823 K. And the higher
hardness with the holding temperature of 823 K is due
to relatively higher temperature resulting in the dissol-
ution of overaging strengthening particles. The increasing
hardness of the nugget is related to complete solution of
overaging strength phases and new precipitation of fine
needle-shaped precipitates. With the holding temperature
of 823 K, the precipitates are very fine and seem to be uni-
formly distributed throughout the matrix. This is the main
reason for the enhanced hardness.
Conclusions
The Al–Mg–Si aluminium alloy with T6 temper was self-
support friction stir welded. The performance and micro-
structure evolution is investigated with post-weld heat
treatment. Increasing the annealing time, the strengthen-
ing-phase particles occurred dissolving and coarsening.
The hardness decreased from average 59 to 52HV with
holding time from 10 to 60 minutes at temperature 723
K. With increasing the holding temperature, the micro-
hardness tends to be uniform and increased due to com-
plete solution of overaging strengthening particles and
new precipitation of fine needle-shaped precipitates. The
weld nugget grain with shoulder action undergoes abnor-
mal grain growth depended on holding temperature and
intense plastic deformation.
Acknowledgements
The work was supported by the National Natural Science
Foundation of China (No. 51575132).
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