Materials Science & Engineering A 609 (2014) 147–153

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Materials Science & Engineering A

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

Effects of deep cryogenic treatment and low-temperature aging on the

mechanical properties of friction-stir-welded joints of 2024-T351
aluminum alloy
Ji Wang a,b, Ruidong Fu a,b,n, Yijun Li a,b, Jianfeng Zhang a,b
a
State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao, Hebei 066004, PR China
b
College of Materials Science and Engineering, Yanshan University, Qinhuangdao, Hebei 066004, PR China

art ic l e i nf o a b s t r a c t

Article history: Low-temperature aging treatments at 120 1C for 8 h, with and without deep cryogenic pretreatments,
Received 16 February 2014 were conducted for friction-stir-welded joints of 2024-T351 aluminum alloys. The microstructures and
Received in revised form mechanical properties of the welded joints after the above treatments were investigated. Two obvious
14 April 2014
soft zones were found to be located at the retreating and advancing sides of the heat-affected zone (HAZ)
Accepted 17 April 2014
in the as-welded joint. After a single low-temperature aging treatment (LTA), the soft regions close to the
Available online 29 April 2014
base metal in the HAZ almost vanished, while the soft regions close to the thermal-mechanical-affected
Keywords: zone were not significantly affected. Moreover, tensile fracture occurred along the segregation bands of
Aluminum alloys the precipitates in the nugget zone (NZ). This resulted in a decrease in the elongation of the as-welded
Friction stir welding
joint from 74% to 38% that of the base metal. After low-temperature aging with a deep cryogenic
Deep cryogenic treatment
pretreatment at 77 K, the features of the soft zones were similar to those in the case of the single LTA, but
Low-temperature aging
Tensile properties the tensile fracture at the segregation bands in the NZ was inhibited. Consequently, the elongation of the
joints improved along with an increase in tensile strength. The possible mechanisms related to the
improvement of tensile properties of the joints were discussed.
& 2014 Elsevier B.V. All rights reserved.

1. Introduction the HAZ, attributable to the dissolution of very fine S phase

particles [2]. The existence of the soft zone not only degrades
Friction stir welding (FSW) is a solid-state joining technique the strength but also elongation of the joints. Therefore, many
that has been successfully applied to the joining of high-strength studies have been conducted to attempt the elimination of such
aluminum alloys, which are difficult to weld by fusion welding soft regions by manipulating the thermal boundary conditions of
methods [1]. Based on the features of the microstructure, several the welded joint [3–5]. For example, Hassan et al. [3] found that
different zones were clarified along the transverse direction of the for a given travel speed, the hardness values of NZ is positively
FSW joint, such as the nugget zone (NZ), Thermo Mechanically proportional to the rotational speed of the tool. Reynolds et al. [4]
affected zone (TMAZ), and heat-affected zone (HAZ). Severe plastic found that the softening in HAZ of FSW aluminum alloy joint can
deformation and high temperatures in the NZ and partial TMAZ be reduced by decreasing the exposed time at temperature of
result in grain refinement, texture development, and dissolution around 350 1C. Fu et al. [5] effectively restricted the softening in
or re-precipitation of precipitates. In the HAZ, only a slight growth the FSW joint of 2024 aluminum alloy by using the parameter
of the grain, and dissolution or coarsening of the precipitates combination of high rotational speed (1500 rpm) and travel speed
occur. The problem related to these variations in the microstruc- (1000 mm/min).
ture is the softening of the FSW joints. For example, Jones et al. In addition, some researchers have attempted to restrict soft-
found that there were two minima hardness zones in the HAZ of ening in the FSW joint by using external forced cooling [6–9]. For
FSW joints for the 2024-T351 aluminum alloy. One minima was example, Upadhyay et al. [6] and Fratini et al. [7] found that water
close to the TMAZ, attributable to the coarsening and over-aging of cooling resulted in higher strength and ductility of FSW joints.
the S phase particles, and the other was close to the outer edge of Detailed researches on FSW in air, cold water (approximately 8 1C),
and hot water (about 90 1C) for a 7050 aluminum alloy was
n
conducted by Fu et al. [8]. The results showed that the mechanical
Corresponding author at: State Key Laboratory of Metastable Materials Science
and Technology, Yanshan University, Qinhuangdao, Hebei 066004, PR China.
property of the FSW joint welded in hot water was the best among
Tel.: þ 86 335 858 7046; fax: þ 86 335 807 4545. the welded joints tested. As mentioned above, either the optimi-
E-mail address: [email protected] (R. Fu). zation of the thermal conditions or external cooling methods

http://dx.doi.org/10.1016/j.msea.2014.04.077
0921-5093/& 2014 Elsevier B.V. All rights reserved.
148 J. Wang et al. / Materials Science & Engineering A 609 (2014) 147–153

reduced the conduction of the thermal flow from the NZ to the The specimens for metallographic analyses and tensile tests
surrounding regions. Consequently, not only the exposed time were cut perpendicular to the welding direction using an
under higher temperature but also the distribution ranges of the electrical-discharge cutting machine. The metallographic speci-
softened zones in the HAZ can be effectively reduced. However, for mens were polished, etched with 25% nitric acid at 75 1C for
the case of the moderate or high weld heat input [10] and a thick  3 min, and then observed by optical microscopy (Axiovert 200
plate joint, these methods proved to be insignificant because of MAT) and scanning electron microscopy (SEM; HITACHI S-3400).
the limitations of the heat conductive capability. Energy-dispersive spectroscopy (EDS) was employed to identify
Although various methods have been developed to avoid soft- the composition of the precipitation particles. To investigate the
ening of FSW joints, post-weld heat treatment (PWHT) is con- evolution of precipitates in the as- and post-welded treatment
sidered effective for removing soft zones, particularly for thick joints, differential scanning calorimetry (DSC) was conducted
plate joints. However, PWHT with solid solution treatment at high using a NETSCH STA449C DSC instrument. Each specimen, 3 mm
temperatures was shown to cause abnormal coarsening of the in diameter and 1.8 mm in thickness, was heated from 298 K to
grains in the NZ, resulting in the property deterioration of the 823 K at a speed of 20 K/min.
joints [11]. Therefore, a single aging treatment without a solid The Vickers microhardness distribution perpendicular to the weld
solution should be the main approach to improve joint properties. direction was measured on a FM-ARS9000 Vickers hardness instru-
Danaf et al. [12] found that increasing the holding time of aging at ment with a load of 200 g and an interval of 0.5 mm. The configura-
175 1C is beneficial for recovering the strength of the FSW joint for tion and size of the tensile specimens were prepared with reference
6082 aluminum alloy. Moreover, the grain in the NZ barely exhi- to the JIS Z2201 standard, and the tensile tests were performed on a
bited the tendency for abnormal grain growth. Nevertheless, the servo-hydraulic mechanical testing system at a tensile speed of
initial microstructure of the as-welded joint must be considered in 2.4 mm/min. The fracture surfaces were examined by SEM.
the single aging treatment. For example, if the microstructure of a
zone in the joint is just at the peak-aging state, high-temperature
aging treatment may degrade the property of the joint owing to 3. Results
over-aging effects.
Currently, deep cryogenic treatment (DCT) is mainly used in 3.1. Microstructures of the as-welded FSW joints
alloy steels to further modify the microstructure [13]. There are
several theories concerning the effects of DCT in published papers. The metallographic microstructures on the cross section of the
One is the deep cryogenic environment will cause the decreasing as-welded joint are shown in Fig. 1. From the overall observation
of point defects and the increasing of dislocations density in the shown in Fig. 1a, the FSW joint is conventionally divided into four
crystal. Another one is the nearly-complete transformation of regions, i.e., the NZ, TMAZ, HAZ, and base metal (BM). The larger and
retained austenite into martensite in steels. Besides, the elevated elongated grain structures parallel to the rolling direction (see Fig. 1b)
internal energy can also promote the fine dispersed carbides in the BM were replaced by a mount of refined grains in the NZ
precipitation. (see Fig. 1c). This is attributed to the dynamic recrystallization caused
While only few works have been conducted for the effect of by severe thermal plastic deformation in the NZ. A mixture of
DCT on the aluminum alloys [14–16]. Chen et al. [17] system- coarsened and refined grains in the TMAZ was typical because of
atically studied DCT for several aluminum alloys and found that the incomplete dynamic recovery and recrystallization in this zone
the strength of the DCT sample at room temperature enhances but (see Fig. 1d). The TMAZ is a transitional region between the NZ and
ductility decreases. The exception is for 6063 aluminum alloy, in HAZ. The width of this transitional region is narrower on the
which the strength decreases but elongation increases. In addition, advancing side than on the retreating side. The grain size in the
numerical simulations proved that the decrement rate of the HAZ (see Fig. 1e) was not different from that in the BM. This is
residual stress is approximately 58% for the DCT of 7050 aluminum because the thermal affection is insufficient to modify the initial grain
alloy [18]. Qian et al. [19] found that the pre-aging effect resulting structure of the HAZ. Normally, the coarsening or dissolving of
from DCT promotes the precipitation of the second phases for precipitates causes the major variations in the microstructure of the
ZL201 aluminum alloy. In comparison, there are few reports on the HAZ. The detailed variations in the microstructures and their effects
application of DCT to FSW joints. on the performance of FSW joints are discussed later.
In this study, the effects of PWHT combined with DCT with low-
temperature aging were investigated on the FSW joints of 3.2. Hardness distribution
2024-T351 aluminum alloy. The conceivable mechanism of DCT
and low-temperature aging treatment are discussed. The hardness distributions of the four joints under different
treatment states are shown in Fig. 2. In FSW joints of high-strength
aluminum alloys, the minima hardness zones are always those in
2. Experimental procedures which precipitates occur with notable variation due to the weld heat
effect. Under the present welding parameters, although a high peak
2024-T351 aluminum alloy sheets with a gauge thickness of temperature resulted in high hardness in the NZ, softening was
2 mm were employed. Their nominal compositions are 4.3% Cu, inevitable in the FSW joints. There were two obvious soft regions
1.6% Mg, 0.7% Mn, and the balance Al. Sheets with a width of (labeled I and II in Fig. 2) in the HAZ on both the advanced and
60 mm and length of 150 mm were butt welded on an FSW retreating sides for the as-welded joint. The same result has been
machine (FSW-3LM-2010). The stir tool with a shoulder and pin reported by Jones et al. for the FSW joint of 2024-T351 aluminum
was made of H13 steel. The diameters of the threaded pin and tool alloy [2]. These soft zones had almost no variation after post-welded
shoulder were 1.9 mm and 10 mm, respectively. The travel and treatment by single DCT. However, after the post-welded LTA
rotational speeds of the tool were 200 mm/min and 1500 rpm, treatment at 120 1C for 8 h, soft zone Ι (SRΙ) vanished, while the
respectively. The tilt angle of the tool was 21. minima hardness in the soft zone ΙΙ (SRΙΙ) increased. Similarly, the
Three different treatments were conducted immediately after hardness in SRΙ increased in the same way with the post-welded
welding: low-temperature aging (LTA) treatment at 120 1C for 8 h, DCA; however, the minima hardness in SRΙΙ did not vary with the
DCT at  196 1C for 24 h, and DCT combined with low-temperature expected amplitude. This smaller increment implies an effect result-
aging treatment (DCA). ing from DCT prior to LTA.
 J. Wang et al. / Materials Science & Engineering A 609 (2014) 147–153 149

b e d c

Advancing side Retreating side 2mm

Fig. 1. Metallography on the cross-section of the joints: macrostructure of the joints (a), microstructures of the base metal (b), NZ (c), TMAZ (d) and HAZ (e).

180 Rp0.2
1500-200
TMAZ

450 Rm 14
A [%]
170 BM HAZ NZ 1500-200-DCT
1500-200-DCA 400 12
Vickers hardness (HV)

160 1500-200-A 350

I II 10

Elongation [%]
300
150
Strength [MPa]

250 8

140 200 6
150
130 4
100
120 Retreating side Advancing side 2
50

0 0
110 BM 1500-200 DCT DCA LTA

-20 -15 -10 -5 0 5 10 15 20 Sample

Distance from the central line (mm) Fig. 3. Comparison of the tensile properties of the joints under different treatment
conditions. Rp0.2: yield stress (MPa), Rm: ultimate tensile stress (MPa), A [%]:
Fig. 2. Hardness distribution of the joints under different treatment conditions. elongation.

3.3. Tensile performances

In comparison, both UTS and elongation of the single DCT joint
Fig. 3 shows the comparison of tensile properties among the slightly decreased compared with those in the as-welded joint.
FSW joints after different post-welded treatments. The UTS of the Similarly, for the single LTA joint, the strength decreased to
as-welded joints was 458 MPa, which is 96.3% that of the BM 426 MPa, which is approximately 90% that of the BM, and the
(476 MPa). Meanwhile, elongation was nearly 74% that of the BM. elongation decreased to 38% that of the BM. However, UTS and
150 J. Wang et al. / Materials Science & Engineering A 609 (2014) 147–153

Retreating side Advancing side

Retreating side Advancing side

Retreating side Advancing side

Retreating side Advancing side

Fig. 4. Fracture locations of the tensile samples for the as-welded joint (a), and joints with DCT (b), DCA (c) and LTA (d).

especially elongation of the DCA joint improved significantly; microstructure, which strongly depend on the weld heat input
elongation increased to 80.2% that of the BM. condition. In the HAZ, weld heat often causes grain growth and
Fracture location observation results (as shown in Fig. 4) dissolution or coarsening of precipitates. As a result, softening in
indicate that the as-welded joint (see Fig. 4a), DCT joint (Fig. 4b), the HAZ is inevitable, especially when the GP zones are the main
and DCA joint (Fig. 4c) fractured at SRΙΙ on the retreating side of strengthened phase in T351 tempered microstructure of 2024
the joint. The crack path was nearly 451 from the normal direction aluminum alloys.
of the welded plate. This is a typical shearing fracture mode often Fig. 6 shows the DSC analysis results of the precipitates under
encountered in the plate tensile test. However, the abnormal different post-weld treatments in the SRI. An endothermic peak
fracture occurred at the NZ near the advancing side of the LTA (labeled Ι) was observed near 150 1C in the DSC curve, which is
joint. Moreover, the crack feature at the upper position of the NZ attributed to the dissolution of the GPΙ zone. Another endothermic
was smooth (see Fig. 4d). peak (labeled ΙΙ) was observed at 240 1C, which is attributed to the
Further observations of the fracture surfaces of the above joints dissolution of the unstable phases, such as the GPΙΙ zones or the S″
are shown in Fig. 5. For the specimens' fracture at SRΙΙ on the unstable phase. On the other hand, the two endothermic peaks
retreating side of the joint, the fracture surface exhibited similar overlap with each other, implying that the structures of the GPΙ
features, which were composed of cleavage planes and small and GPII zones are similar [20]. Based on the calculation of the
dimples (see Fig. 5a–c). However, for the specimen fracture at peak area under the DSC curve, we can deduce the total volume
the NZ, a smooth surface feature, which corresponds to the crack fraction of the GPΙ and GPΙΙ zones before DSC heating, i.e., the
position in Fig. 4d, was easily distinguished at the upper position as-treated specimens. The larger the area, the greater the volume
of the fracture surface (see Fig. 5d). We can deduce that this fraction of the GP zones in the as-treated specimens [21]. The
fracture surface may be closely involved with the segregation of exothermic peak near 270 1C (labeled ΙΙΙ) is attributable to the
the microstructure, particularly the precipitates. precipitation of the S0 or stable S phases. However, the S0 phase
cannot be easily distinguished from the S phase and thus is
regarded as the same as the S phase. Assuming minimal over-
4. Discussions lapping of endothermic and exothermic heat flows between GP
zones transforming to the S phase and the dominance of the
4.1. Microstructure evolution of soft regions formation energy over other factors such as coarsening, the peak
area at the region labeled II corresponds to the amount of the S
The hardness distribution of an FSW joint of a heat-treatable phase transformed at the expense of the GPB zone during the DSC
strengthening aluminum alloy is close to the variations of the experiment, which is complementary to the amount of the S phase
 J. Wang et al. / Materials Science & Engineering A 609 (2014) 147–153 151

Fig. 5. Fracture surfaces of the tensile samples for the as-welded joint (a), and joints with DCT (b), DCA (c) and LTA (d).

0.15 such a small infraction of the GPΙ zone is not sufficient to cause
1500-200-SRI the obvious variation in the hardness of the soft zones. Thus, the
DCT disappearance of the SRI in joints should be contributed to the
DCA
0.10 effect of aging at 120 1C during DCA and LTA.
LTA
The other regions also present similar results but not as
obvious as those in the SRI because of the different initial states.
DSC /(mW/mg)

0.05 For example, the NZ was found to have typically refined grains
III with some unstable phases, which can re-precipitate during the
I
cooling stage or natural aging after FSW and result in a higher
0.00 hardness in the NZ. In addition, the soft mechanism of the SRΙΙ has
II been reported to be the coarsening of the fine S phases [2]. In the
present LTA or DCA treatment results, the hardness in the NZ
-0.05 slightly increases because of further precipitation of the unstable
phases; however, the fraction of the GP zone existing in the SRΙΙ is
too small to cause an obvious increase in the hardness.
-0.10
100 200 300 400 500
4.2. Tensile fracture behavior
Temperature /°C
Fig. 6. DSC analysis of the joints in the SRI under different treatment conditions. The tensile properties and fracture locations of FSW joints are, to
a large extent, dependent on the hardness distribution of the joints.
originally present in the as-treated sample. That implies that the From Fig. 2, both SRI and SRII are the weakening locations of the
more S is transformed from the GP zones, the less is the amount of joints, especially SRII, which has hardness minima in the overall
the original S phase in the as-treated specimens. joints irrespective of the treatments employed. Thus, the tensile
The SRI appears possibly as a result of the dissolution of the GP fracture prefers to occur at the SRII (see Fig. 4a to c). However, it is
zones or the very fine S phase owing to the thermal cycle during notable that the fracture location shifts from the SRII to NZ in the
the FSW [2]. As shown in Fig. 6, the fractions of the GP zones case of LTA (see Fig. 4d). Moreover, the crack feature on the upper
increase in the specimen treated by DCA and LTA. This is mainly position of the NZ appears smooth and may be related to the
because the LTA at 120 1C facilitates the further precipitation of the segregation of the precipitates. To seek the causes of this fracture
GPΙΙ zones in the SRI, increasing the hardness in those regions. feature, a special etched method was employed to highlight the
In comparison, single DCT cannot result in obvious effects on the precipitates in the NZ for joints treated by DCA and LTA.
GP zones. Instead of an increase, a slight decline in the fraction From the SEM observations in Fig. 7, the features of the
of the GPΙ zone can be observed for single DCT. We can deduce segregation bands of the precipitates (shown by arrows) can be
that single DCT accelerates the re-dissolution of the GPΙ zones, but easily distinguished in the NZ of all specimens. Fig. 7a shows the
152 J. Wang et al. / Materials Science & Engineering A 609 (2014) 147–153

(Cnt)
spot A

(keV)

Fig. 7. Observations of the segregation bands in the NZ. (a) The as-welded joint, (b) The EDS results of precipitates located at the spot A as shown in (a), (c) the DCA joint, and
(d) the LAT joint.

distribution of precipitates in the as-welded specimen. The EDS the dispersed precipitation of the unstable phases in the matrix
results of the precipitates at the point (labeled A in Fig. 7a) on the during subsequent LTA. On the other hand, the dislocation density
segregation band indicate that the segregation bands consist of increases because of the lattice shrink at cryogenic temperatures.
Al–Cu phases (see Fig. 7b). The same results were also obtained by This results in enhanced interaction between the vacancies and
Ma et al. for 2024-T3 alloy FSW joint [22]. The existence of the dislocations. Meanwhile, the long distance diffusion of a single
segregation bands in the NZ can cause a crack along these regions solute atom is difficult under the present aging temperature
at lower stress levels. Accompanied by grain refinement in the NZ, condition, and the solute atom and vacancy prefer to constitute
the precipitates can form segregation bands, which are related to a diffusion couple. Thus, the migration of the solute atoms largely
the diffusion of the alloy elements under the cooperative effects of depends on the diffusion capability of the vacancies. In the
the larger gradient of the strain or strain rate and weld heat subsequent LTA process, although lattice expansion occurs, result-
during FSW. ing in the regeneration of the vacancies, the solute atom–vacancy
After DCA treatment, the segregation bands become thinner diffusion couples cannot migrate a long distance because of high-
and shorter. Meanwhile, the distribution of the precipitates density dislocations. However, these diffusion couples can easily
appears to be more dispersed and uniform (Fig. 7c). On the migrate to the segregation bands since there are few dislocation
contrary, the more serious segregation can occur in the NZ when obstacles after dynamic recrystallization in the single LTA NZ.
treated by a single LTA (Fig. 7d). In fact, the microstructure in the Consequently, the overall tensile performance of the FSW joint
NZ is often considered an incomplete aging state. This indicates treated by the DCA improves.
that the unstable phase particles will continuously precipitate at
moderate thermodynamic conditions after FSW. Therefore, the LTA
promotes the precipitation process of the unstable phases at the 5. Conclusions
existing segregation bands. On this account, a pre-DCT was
performed before LTA in the process of DCA. The pre-DCT results (1) Two types of soft regions exist in the HAZ of the as-welded
in shrinking weld volume. Consequently, it leads to the decrease joint: SRI and SRII. Both DCA and LAT can remove the SRI, but
in the vacancy density and increase in the dislocation density. not the SRII, with the minima hardness.
The above processes effectively weaken the segregation extent in (2) After treatment by the single LTA, the elongation of the as-
the NZ during the subsequent LTA. The detailed processes can be welded joint dramatically decreased and was accompanied by
explained as follows: the compressive strain resulting from the a small decrement in the strength. The tensile fracture location
lattice shrink may lead to the re-precipitation or re-dissolution of shifted from the SRII of the as-welded joint to the NZ of the
unstable precipitates with coherent or semi-coherent lattices in LTA joint. This indicated that a single LTA does not improve the
the matrix. These processes may also occur at the regions near the tensile property of the as-welded joint but deteriorates it.
segregation bands. This may not only reduce the tendency of the However, an enhanced tensile property was achieved using
solute atoms to migrate to the segregation bands but also promote DCA, in which a pre-DCT was employed before the LTA.
 J. Wang et al. / Materials Science & Engineering A 609 (2014) 147–153 153

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