Materials Science & Engineering A 754 (2019) 728–734

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Materials Science & Engineering A

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

Effect of post-weld heat treatment on the mechanical behavior and T

dislocation density of friction stir welded Al6061
Amir Hossein Baghdadi∗∗, Armin Rajabi, Nor Fazilah Mohamad Selamat, Zainuddin Sajuri∗,
Mohd Zaidi Omar
Centre for Materials Engineering and Smart Manufacturing, Faculty of Engineering and Built Environment, Universiti Kebangsaan Malaysia, 43600, UKM Bangi, Selangor,
Malaysia

A R T I C LE I N FO A B S T R A C T

Keywords: Al6061 is a heat-treatable aluminum alloy and an extremely versatile material used in settings where medium to
Al6061 high strength is required. To produce good joints using this alloy, a particular solid-state welding process called
FSW friction stir welding (FSW) is preferable instead of the conventional welding methods. In this study, the effects of
PLC T6 post-weld heat treatment (PWHT) on the mechanical properties, dislocation density, and microstructure of a
Precipitation hardening
friction stir welded (FSWed) Al6061 aluminum alloy were investigated. Results indicated that FSW had degraded
XRD
the mechanical properties of Al6061. The welding efficiency decreased to 65% compared with the tensile
Dislocation density
strength of the base metal. After FSW, the samples demonstrated a serrated flow behavior known as the
Portevin–Le Chatelier (PLC) effect. This effect was attributed to the nonuniform distribution of hard Mg2Si
particles, coarsening and/or solutionizing of the strengthening elements in the stir and thermomechanically
affected zones, and an over-aging effect in the heat-affected zone of the FSWed sample. However, the T6-PWHT
performed on the FSWed sample diminished the PLC effect and concurrently improved the mechanical prop-
erties back to its original state. The PWHT also promoted precipitation hardening through a better distribution of
Mg2Si particles that prevented grain growth and increased the dislocation density due to the applied strain,
which subsequently improved the mechanical properties of the FSWed Al6061 alloy.

1. Introduction dissolution or loss, porosity formation, and grain coarsening [6–10].

Aluminum (Al) alloys are widely used in the construction and
transportation industries because of their good mechanical properties,
including high specific strength, high toughness, corrosion resistance,
light weight, and recycling capabilities [1]. 6xxx series aluminum alloys
are extremely versatile and multipurpose aluminum alloys that are heat
treatable. These alloys are typically utilized in settings where medium
to high strength and good toughness properties are required, such as
components for transportation, equipment and machinery, consumer
durables, and recreational goods. Furthermore, the Al6061 aluminum
alloy has been utilized in the automotive industry [2], marine frames
and pipeline, and aircraft [3]. Magnesium and silicon are the major
alloying elements [4] for this grade of Al alloy. The strength of Al6061
increases via precipitation hardening of these alloying elements [5].
Welding is an essential manufacturing process used for a wide
variety of aluminum-based products. However, fusion welding pro-
cesses for joining Al alloys lead to several problems, such as precipitate
Moreover, age-hardened grades may be subject to cracking after
welding. Friction stir welding (FSW), a joining technique in the solid
state, could be the best alternative method to join Al alloys [11,12].
FSW provides several advantages, including high-quality joints, precise
external control and repeatability at high levels, lack of special sample
preparation, low-energy process, and low pollution. Moreover, FSW
works by deforming the material below melting point temperatures,
resulting in reduced distortion and residual stress problems [13].
After the FSW process, an alteration typically occurs in the me-
chanical properties and microstructure of aluminum alloys due to the
increased temperature of the base material during the welding process.
These alterations could be the reason for the lack of strength in the
material. The as-welded alloy showed repeated or serrated yielding
during the tensile test, thereby indicating that a plastic instability ex-
isted related to the discontinuous plastic flow and inhomogeneity of the
plastic strain. This behavior is known as the Portevin–Le Chatelier
(PLC) effect [14]. The PLC effect has been observed in many metallic

∗
Corresponding author.
∗∗
Corresponding author.
E-mail addresses: baghdadi.amirhossein@gmail.com (A.H. Baghdadi), zsajuri@ukm.edu.my (Z. Sajuri).

https://doi.org/10.1016/j.msea.2019.03.017
Received 14 September 2018; Received in revised form 2 March 2019; Accepted 4 March 2019
Available online 07 March 2019
0921-5093/ © 2019 Elsevier B.V. All rights reserved.
A.H. Baghdadi, et al.
solid solutions, particularly in Al-based lightweight alloys. This effect
arises when plastic deformation is carried out in a certain temperature
range, loading rate, and strain [14–17]. Discontinuities in the flow
stress that make up the PLC effect are widely believed to have origi-
nated from a dislocation scale caused by the interactions between
mobile dislocations and solutes. These effects are strongly determined
by many different factors, including spatial distribution of atoms and
their solute concentration, grain size, initial dislocation structure, and
activation energy that unlocks the dislocations “arrested” at pre-
cipitates or in the dislocation structures [18–20]. Several models have
been used to explain the PLC process [20–22], and a common point of
agreement centers around it being attributed to the jerky dislocation
motion and the flow pattern that becomes serrated as a result. More-
over, the PLC process is attributed to the interaction of dynamic solute
atom and dislocation, which occurs as a result of hindering the dis-
location motion by solute atoms that have been segregated at the core
of the dislocation.
The problem described above can be solved by performing heat
treatment on the part that needs to produce the desired mechanical
properties and to also relieve the residual stress of the welded area [3].
A number of cooling and heating procedures are incorporated into the
heat treatment process, which is conducted to create changes in a
material's microstructure that will in turn affect its mechanical prop-
erties. In other cases, strain hardening effects that occur during for-
mation can be relieved by heat treatment so that the material can be
subjected to further deformation [23]. The three main processes used
for the heat treatment of 6xxx series aluminum alloys are as follows:
solution heat treatment, quenching, and aging [24]. PLC behavior has
high microstructure sensitivity and is significantly affected by grain
refinement, which can also influence the mechanical behavior of Al
alloys [18,19,25]. Grain refinement caused by severe plastic deforma-
tion is related to subgrain (dislocation cell) boundary evolution, and the
development of the cell structure is likely to result in strain aging
phenomena [26]. Hence, analyzing the evolution of dislocation density
during FSW is necessary to comprehend the refinement in the micro-
structure and the effect on the behavior of the PLC. Of note, XRD is still
used to indirectly measure the dislocation density because it is faster,
easier, and inexpensive compared with TEM. Dini et al. [27] reported
that the XRD technique would be a reasonable method for the estima-
tion of the dislocation density with regard to tensile-strained TWIP steel
samples. Rajabi et al. [28] also indirectly calculated the dislocation
density of synthesized nano-TiC using the XRD method. Mohamed et al.
[29,30] also investigated the dislocation densities via XRD method to
present the strengthening mechanism of heat treatable Al6061 and
Al2024 aluminum alloys.
Although investigations have been conducted on the effect of post-
weld heat treatment (PWHT) on Al alloy mechanical properties and
microstructure in recent years, systematic investigations on the PLC
effect have seldom been performed on friction stir welded (FSWed)
Al6061 and its mechanical properties and dislocation density. Thus, in
the present work, the effect of PWHT on the PLC effect and mechanical
properties of FSWed samples will be analyzed and discussed, and the
dislocation density will be calculated.
2. Methodology
This study used commercial Al6061 (T6) aluminum alloy with a
dimension of 150 mm × 50 mm × 4 mm as the base metal. Table 1
presents the compositions of the alloy used and its mechanical prop-
erties. Prior to FSW, surface oxides were removed using a steel brush
and then cleaned with acetone. A cylindrical threaded M5 pin made
from a heat-treated H13 steel tool with a hardness of 53–55 HRC was
used as the FSW tool. Fig. 1(a)–(c) show the schematic of the joint
design, sample dimensions, and FSW tool pin used at a 3° tilled angle of
tool axis during the welding process, respectively. The plunge depth
was constant at 0.3 mm during the welding process. The tool rotational
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Materials Science & Engineering A 754 (2019) 728–734
Table 1
Chemical compositions and mechanical properties of the material used.
Material Chemical composition (wt. %) Yield Ultimate
stress tensile
Al Mg Si Mn Cu (MPa) strength
(MPa)
Al6061(T6) Balance 0.8 0.4 0.03 0.18 246 279
speed and traveling speed were 1200 rpm and 100 mm/min, respec-
tively. Two sets of joints were made so that the effect of PWHT on the
mechanical properties of the samples could be determined: one as-
welded (FSWed) sample and one heat-treated (PWHTed) sample. The
PWHT process consists of solutionizing and artificial aging at 535 °C for
1 h and 175 °C for 8 h, respectively.
Microstructure observation of both samples was performed on the
cross-sectional weld area perpendicular to the welding direction. An
etching solution consisting of 1.5 ml hydrochloric acid, 2.5 ml nitric
acid, 1 ml hydrofluoric acid, and 95 ml distilled water was used to de-
termine the microstructure of Al6061(T6) in different welding regions.
The microstructure was observed under an optical microscope. The
average grain size of both samples was then measured based on the
ASTM standard E112-10. The tensile test was performed on a Zwick/
Roell tensile test machine with a 100 kN capacity at an ambient tem-
perature (25 °C) and cross-head speed of 1 mm/min (strain rate 10−3).
The specimen used for the test had a length and width of 100 mm and
10 mm, respectively.
After welding, the joined plates were cut into a dog bone shape
tensile test specimen perpendicular to the welding direction. To de-
termine the effect of PWHT on the evolution of dislocation density of
FSWed Al6061, the tensile samples were strained at a constant strain
rate at the start and then at different strain percentages of 1%, 2%, 4%,
6%, and 11% (the maximum at the UTS point) for the FSWed and
PWHTed samples. All samples were further analyzed using XRD to
identify the dislocation density. XRD analysis was conducted using a
Bruker AXS Germany diffractometer with monochromatic Cu–Kα ra-
diation (λ = 0.1541 nm) at 40 kV and 4 mA.
3. Result & discussion
3.1. Microstructure
Fig. 2 illustrates that the as-received Al6061 plate had an elongated
microstructure of inhomogeneous grains that possessed an average
grain size of 32 μm. A considerable amount of round and rodlike par-
ticles, which had not been homogeneously distributed at the grain
boundaries, were present. These particles were believed to be Mg2Si
[31]. Fig. 3 shows the different cross-section magnifications of the
samples under FSWed and PWHTed conditions.
Fig. 3(a) shows the different welding zones that make up the FSW as
follows: stir zone (SZ), thermomechanically affected zone (TMAZ), and
heat-affected zone (HAZ). This figure illustrates that the grain size of SZ
is smaller than that found in TMAZ and HAZ due to the severe plastic
deformation and higher frictional heat input imposed on these areas as
a result of the tool shoulder and tool pin [32].
Fig. 3(b) and (c) reveal the respective SZs of the FSWed and
PWHTed samples. The SZ grains of the FSWed sample exhibited
boundaries that were slightly corrugated. The corrugation might be
attributed to the nonuniform distribution of dislocations due to a higher
rotation speed that subsequently caused higher plastic deformation.
Some researchers [26–28] have also reported that grain evolution tends
to become corrugated while materials are being hot worked because the
absorption capacity of the grain boundaries is exceeded by the density
of dislocations entering them or when an incubation time is required by
the lattice dislocation process (requires a lengthy time).
A.H. Baghdadi, et al.
Fig. 1. (a) Experimental setting, (b) sample dimensions, and (c) FSW tool.
Fig. 2. Microstructure of the as-received Al6061(T6).
During the FSW, the welded plates experience heat input caused by
the annealing effect, thus leading to the coarsening and/or solutio-
nizing of the strengthening elements in the SZ and TMAZ [3]. Fur-
thermore, HAZ could be subjected to an over-aging effect caused by the
coarsening of strengthening elements due to heat input prior to being
joined. Fig. 3(c) shows the positive effect on the microstructure of the
FSWed sample after PWHT. PWHT caused the homogeneous distribu-
tion of the strengthening particles in the SZ compared with the SZ of the
FSWed sample. Moreover, the grain size in the SZ of the PWHTed
sample was slightly coarser than the as-welded sample due to the so-
lutionizing process.
3.2. Tensile properties
Fig. 4 represents the stress–strain curves of FSWed samples in both
as-welded and PWHTed conditions. As shown in the figure, a significant
improvement in the mechanical properties can be noted after the heat
treatment. However, the welding efficiency obtained for the FSWed
sample was around 65%, which was calculated from the ratio of the
ultimate tensile strength (UTS) values of welded samples to the base
material. The low UTS value of the FSWed sample could be attributed to
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Materials Science & Engineering A 754 (2019) 728–734
the coarsening and/or solutionizing of the strengthening elements in
the SZ and TMAZ and the over-aging effect in the HAZ of the FSWed
sample [26,29–32].
In the PWHTed sample, the UTS reached up to 316 MPa. An increase
in elongation from 10.9% in the FSWed sample to 16% in the PWHTed
sample was noted. The changes in tensile stress behavior of the FSWed
sample would be consistent with the idea of a nonuniform distribution
of hard particles (Mg2Si) in the Al matrix (Fig. 3(b)), resulting in the
serrated flow pattern shown in Fig. 4. However, no serrated behavior
was observed in the stress–strain curve of the PWHTed sample. These
results suggest that the uniform plastic flow followed those subjected to
a regular form and good uniform distribution of the precipitation
hardening in the matrix.
Generally, plastic deformation is accompanied by the relative
sliding of atomic planes in an organized manner in crystalline solids.
During the slip, each atom typically moves in the same integral number
of atomic distances along the slip plane producing a step, but the or-
ientation of the crystal remains the same. Slip planes are typically the
closest packed planes, that is, the planes with maximum atomic density,
and they significantly contribute to the overall extension of a tensile
specimen [33].
Slip occurs as a result of the motion of dislocations from one place to
another with the accumulation of stress. The dislocations can be fa-
vorably nucleated at the grain boundaries, thus hardly traversing the
grain interior. Dislocation pile-up might continue and accumulate at the
grain boundaries, thereby increasing the mechanical properties. T6 heat
treatment, which also includes solution and artificial aging treatments,
improves the mechanical properties due to the hardening effect of
precipitation. The precipitates interact with dislocations affecting the
material behavior during the tensile test, which causes a higher shear
stress to be required to move the dislocations. Therefore, increasing the
flow stress is crucial to maintain an imposed strain value that will either
generate new dislocations or unlock the dislocations from obstacles.
The rate of dislocation density was investigated using the XRD experi-
ment results from the beginning tensile test (1% strain) up to the UTS in
the FSWed and PWHTed samples. Fig. 5 shows the XRD patterns of the
FSWed and PWHTed samples.
The dislocation density ρ (per m2) can be evaluated using the
microstrain < η2 > 1/2, Burgers vector (B) and average crystallite sizes
(d) from the XRD data. For the FCC structure, the Burgers vector is B =
A.H. Baghdadi, et al. Materials Science & Engineering A 754 (2019) 728–734

Fig. 3. (a) Higher magnification of the welding zone, (b) & (c) Higher magnification of SZs under the FSWed and PWHTed conditions, respectively.

Fig. 4. Stress-strain curves of the joints in both as-welded and PWHTed con-
ditions.

a
2
[34] and (a) is the lattice parameter. Then, the equation in Ref. [35]
can be presented as follows:
1
2 3 < η2>2
ρ=
d×B (1)

The Williamson–Hall method was used, after correcting the broad-

ening obtained from the lanthanum hexaboride, to investigate the
change of the crystallite size and microstrain and determine the full
width at half maximum (FWHM) intensity of the selected peak in de-
grees (rad) [36]:
Fig. 5. XRD patterns of samples after tensile test; (a) FSWed, (b) PWHTed.
FWHM = ((FWHM)2Measured e (FWHM)2Instrument )1/2 (2)
Cu–Kα radiation (λ = 0.1541 nm), respectively. Table 2 shows the
According to a linear fitting of the Williamson–Hall plot shown in
crystal size (d) and lattice strain (η) calculated for the samples under
Fig. 6(a) and (b), an average of the crystallite size (d) can be computed
FSWed and PWHTed conditions.
from the y-intercept and the microstrain (η) from the slope using the
Therefore, an increase in applied strain during the tensile test is
following equation [37,38]:
accompanied by an increase in the crystal size and strain of the lattice
0.9λ for the FSWed sample. The decrease in the strain of the lattice with
FWHM × cos θ = + 2η sin θ
d (3) degrees of crystal size was observed in Table 2 at an applied strain of
4% for the PWHTed sample due to precipitation hardening. When
where θ and λ are Bragg's angle of diffraction and the wavelength of

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A.H. Baghdadi, et al. Materials Science & Engineering A 754 (2019) 728–734

Fig. 6. Crystallite size and microstrain of welded samples based on the

Williamson–Hall method; (a) FSWed, (b)PWHTed.

Fig. 7. Determination of lattice parameter of the welded samples using Nelson-

Table 2
Riley method; (a) FSWed, (b) PWHTed.
Mean crystallite size and microstrain amount of the welded samples at different
strain values of the tensile loading based on the Williamson–Hall equation.
Table 3
Sample Applied strain % Y = ax + b d (nm) η (%)
The calculation of dislocation density based on equation (1) in FSWed and
a b PWHTed conditions.
−11
Sample Strain (%) a (Nelson–Riley method) B (10 m) ρ × 1014
FSWed 1 0.0008 0.0021 66 0.08
(Å) (m−2)
2 0.0011 0.002 69 0.11
4 0.0019 0.0015 92 0.19
FSWed 1 4.0518 2.86506 1.46461
6 0.0032 0.0007 198 0.32
2 4.0521 2.86527 1.9178
PWHTed 1 0.0011 0.0019 73 0.11
4 4.0520 2.8652 2.48448
2 0.0026 0.0018 77 0.26
6 4.0516 2.86491 1.95291
4 0.0014 0.0029 47 0.14
PWHTed 1 4.0505 2.86414 1.82028
6 0.0017 0.0027 51 0.17
2 4.0509 2.86442 3.99725
11 0.0038 0.0012 115 0.38
4 4.051 2.86449 4.07553
6 4.0531 2.86597 3.53378
11 4.0547 2.86711 3.9674
pulled, the crystal size/particle resulted in the fractured hard phase
during the tensile test, which, in turn, increased the crystal size and
strain of the lattice as can be observed in Table 2. and (b) show changes in the lattice parameter values with increasing
Once the samples were subjected to the tensile load and microstrain- tensile strain. Table 3 depicts the lattice parameters (a), Burgers vector
induced disturbances, the lattice parameter of Al deviated from the (B), and dislocation density (ρ) values for the samples under FSWed and
database of FCC (a = 0.4094 nm [39]), changing the Burgers vector (B). PWHTed conditions.
To overcome this problem, the Nelson–Riley method was used to obtain Fig. 8 shows the dislocation densities of the samples based on
the Al lattice parameter as follows [40,41]: Equation (1) by considering all the aspects mentioned above. Using the
linear least squares method, the rate of dislocation density was calcu-
1 ⎛ cos2 θ cos2 θ ⎞ lated for the samples using the following equation [27]:
F (θ) = ⎜ + ⎟

2 ⎝ sin θ θ ⎠ (4)
ρ = ρ0 + K.ε (5)
where F(θ) is the Nelson–Riley function and θ is the Bragg angle. The
lattice constants can be obtained from the lattice parameters of dif- where ρ0 is the dislocation density for zero lattice strain and K is the
ferent (hkl) reflections of the FCC crystal structure of aluminum, and dislocation rate.
these were plotted against the Nelson–Riley function with the y-inter- The dislocation density of PWHTed samples increased and reached
cept being used for the value of the accurate lattice parameter. Fig. 7(a) nearly 13.78% compared with that of FSWed samples. Mg and Si are the

732
A.H. Baghdadi, et al.
Fig. 8. Accumulation rate of dislocation density for the samples in FSWed and
PWHTed conditions.
essential strengthening elements applied in Al alloys, which subse-
quently generated precipitation hardening phenomenon in the matrix,
leading to larger increments in strength with only a minimal reduction
of the break elongation [42]. As noted, the T6 treatment on the samples
could create a precipitation hardening phenomenon with better uni-
form distribution in the matrix than FSWed samples (Fig. 3(c)). This is
because the precipitation hardening phenomenon is associated with
grain growth control disrupting movement dislocation, which may in-
teract and lead to increased dislocation value.
4. Conclusion
The effects of T6 PWHT on the mechanical properties, dislocation
density, and microstructure of FSWed Al6061 aluminum alloy were
investigated. The results showed that the FSW process degraded the
mechanical properties of Al6061. After FSW, the welding efficiency
decreased to 65%, and the samples demonstrated a serrated flow pat-
tern known as the PLC effect. These patterns were attributed to the
nonuniform distribution of hard Mg2Si particles, coarsening and/or
solutionizing of the strengthening elements in the SZ and TMAZ, and
the over-aging effect in the HAZ of the FSWed sample. However, the
introduction of T6 PWHT after FSW diminished the PLC effect and si-
multaneously increased the mechanical properties of the Al6061 back
to its original state. The PWHT also promoted precipitation hardening
through better distribution of Mg2Si particles that prevented grain
growth and increased the dislocation density due to the applied strain,
which improved the mechanical properties of the FSWed Al6061 alloy.
Acknowledgement
The authors would like to thank Universiti Kebangsaan Malaysia for
supporting this research project through research funding (AP-2015-
016).
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