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j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4

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

Original Article

Softening behavior of stationary shoulder friction


stir welded joint for thick-plate AleLieCu alloy

Chao Gu, Xinqi Yang*,1, Wenshen Tang, Ting Luo, Ruilin Wang
Tianjin Key Laboratory of Advanced Joining Technology, School of Materials Science and Engineering, Tianjin
University, Tianjin, 300354, China

article info abstract

Article history: 12-mm-thick AleLieCu alloy plates were fabricated by stationary shoulder friction stir
Received 6 July 2022 welding (SSFSW) to evaluate the softening behavior of the whole joint under a given
Accepted 12 August 2022 rotational speed of 400 rpm and a welding speed of 60 mm/min. Continuous dynamic
Available online 27 August 2022 recrystallization, discontinuous dynamic recrystallization, and geometric dynamic
recrystallization are the main dynamic recrystallization mechanisms in SSFSWed joints.
Keywords: Such mechanisms help to gradually change rolling grains of base material (BM) into
AleLi alloy equiaxed grains of welding nugget zone (WNZ) and significantly lower dislocation density.
Thick plates The decrease in dislocation density is the main reason for joint softening. Continuous
Stationary shoulder friction stir coarsening of T1/q0 in heat affected zone (HAZ) and thermo-mechanically affected zone
welding (TMAZ) weakens the strengthening effect. The development of precipitate-free zones and
Softening behaviors re-precipitation of TB primarily contribute to severe softening at the interface between HAZ
Microstructure and TMAZ on the advancing side (AS-HAZ-TMAZ). The serious softening behavior at the
Tensile behavior bottom of WNZ is attributed to the re-precipitation of TB and the complete dissolution of
T1/q0 . Hardness profiles and tensile strength distribution of SSFSWed joint exhibit a “W”
pattern, while a “U” pattern appears at the bottom. The hardness profile and tensile
strength of WNZ are significantly poorer at 8e12 mm from the weld surface compared to
those at 0e8 mm. Softening behavior also results from the higher fractions of the
maximum Schmid factor (in 0.4e0.5) and Cube. From BM to WNZ, fracture mode transi-
tions from quasi-cleavage fracture to plastic fracture.
© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY license (http://creativecommons.org/licenses/by/4.0/).

strength, fatigue resistance, and corrosion resistance while


1. Introduction reducing the weight of aerospace vehicles. In the aerospace
industry, it is gradually taking the place of conventional Al
The precipitation-strengthened AleLieCu alloys, especially alloys as a widely applicated structural material [1,2]. How-
the T8-treated 2195 AleLi alloy, exhibit outstanding specific ever, due to higher heat sensitivity and lower melting point,

* Corresponding author.
E-mail address: xqyang@tju.edu.cn (X. Yang).
1
Present address: School of Materials Science and Engineering, Tianjin University, No 135 Yaguan Road, Jinnan District, Tianjin,
300354, China
https://doi.org/10.1016/j.jmrt.2022.08.060
2238-7854/© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://
creativecommons.org/licenses/by/4.0/).
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4 3009

AleLi alloy components manufactured by fusion welding still 6061-T6 sheets revealed that SSFSWed joints had a more
have to address a number of challenges, such as hydrogen symmetrical and homogeneous microstructure [24]. SSFSW
porosity, thermal cracking, and casting microstructure, which was found to have significantly lower heat input and torque
seriously impair mechanical properties [3,4]. The develop- in the 2-mm-thick dissimilar 2024-T3 and 7050-T651 sheets,
ment of conventional friction stir welding (CFSW) avoids the with a significantly higher SSFSWed joint coefficient (94%)
melting of AleLi alloys during welding. In addition to effec- than CFSWed joints (86%) [25]. However, recent research has
tively eliminating welding defects, it is possible to replace the concentrated more on SSFSW traditional Al alloy sheets such
casting microstructure of the weld zone with fined equiaxed as 5 mm 7075-T651 and 6061-T6 [24,26]. Only one relevant
grains [5,6]. During CFSW, the shoulder and stir pin simulta- research, which primarily investigated the microstructure
neously rotate and glide over the surface to form the weld, heterogeneity along plate thickness and the precipitate
releasing frictional heat that may account for 70e80% of the evolution along the transverse direction, existed for SSFSW
total heat. Therefore, a higher temperature gradient is 1.5-mm thick 2A97 AleLi alloy sheets. The joint coefficient
generated in the stir zone along plate thickness. It produces gradually increased to 78% with the rotational speed
severe residual stress and plastic deformation, and consider- increasing from 600 rpm to 1000 rpm [27]. Studies on soft-
ably increases the heterogeneity of microstructure and me- ening behavior were restricted to WNZ and concentrated on
chanical properties along plate thickness [7,8]. The shoulder CFSW 7.5-mm-thick 2195-T8 AleLi alloy plates and 2-mm-
and stir pin are designed separately in stationary shoulder thick 2060-T8 AleLi alloy sheets. The increase in grain size
friction stir welding (SSFSW) technology. During welding, a and the decrease in dislocation density were generally
stir pin rotates at high speed, squeezing and rubbing the thought to be responsible for softening behavior [28,29]. The
welded material, while the shoulder glides over the weld softening behavior on the whole joint was investigated only
surface without rotating [9,10]. Therefore, SSFSW fundamen- on CFSW 1.8-mm-thick 2198-T8 AleLi alloy sheets. In
tally addresses the problem of excessive heat input on the contrast, the whole joint softening was caused by precipitate
weld surface to obtain more homogeneous microstructure evolution and a decline in dislocation density [30]. Studies on
and mechanical properties along plate thickness, opening up softening behavior, however, did not consider how orienta-
a novel method for welding materials with lower thermal tion factors affected on the HallePetch relationship.
conductivity and thick-plate Al alloys [11,12]. Furthermore, it is necessary to optimize the constant co-
Due to the extremely complex thermo-mechanical efficients of the dislocation density equation for FCC metals
coupling process, SSFSWed joints are separated into four based on the research status of strengthening mechanisms.
zones: base material (BM), heat affected zone (HAZ), thermo- There have not yet been any relevant studies on the soft-
mechanically affected zone (TMAZ), and welding nugget ening behavior in thick-plate AleLi alloy joints fabricated by
zone (WNZ) [13]. Different areas suffer from heterogeneous the innovative SSFSW technology. Microstructure evolution,
temperature histories and plastic deformation, resulting in precipitate evolution, and softening behavior are all gov-
joint softening behavior. Fundamentally, there are four basic erned by both manufacturing technology and plate thick-
factors of joint softening [14]. Firstly, solute atoms such as Cu ness. Consequently, it is essential to carry out SSFSW tests
and Li experience rearrangement and migration when weld- on thick-plate AleLi alloys and investigate thoroughly soft-
ing AleLi alloys. Solute atoms dissolved in solid solutions ening behavior in different areas of the joint.
cause lattice distortion, increasing dislocation resistance and This investigation describes the successful extension of
improving strength and hardness [15]. Secondly, 2195-T8 AleLi alloy experiments to 12-mm-thick plates by the inno-
AleLi alloy exhibits a complicated precipitation system vative SSFSW technology and a self-designed stir tool. The
involving GPZs, q00 (Al2Cu), q0 (Al2Cu), q(Al2Cu), d0 (Al3Li), b0 (Al3Zr), microstructure characteristics, recrystallization mechanisms,
T1(Al2CuLi), TB(Al7Cu4Li), T2(Al6CuLi3). Precipitate evolution and precipitate evolution in the whole SSFSWed joint are
plays a more prominent role in the softening behavior of the systematically expounded. In conjunction with mechanical
joint [16]. Furthermore, the recrystallization mechanism of properties, the softening behavior in different regions of the
CFSWed joints comprises mainly of continuous dynamic whole joint is comprehensively analyzed from the perspec-
recrystallization (CDRX), geometric dynamic recrystallization tives of precipitate evolution, dislocation density distribution,
(GDRX) and discontinuous dynamic recrystallization (DDRX) and the optimized HallePetch relationship. It provides a
[17]. Dynamic recrystallization process reduces the disloca- theoretical foundation for optimizing the SSFSW process for
tion density and leads to joint softening [17,18]. Finally, the thick-plate AleLi alloys, improving joint softening behavior,
relationship between grain size and yield strength is described and manufacturing complex aerospace components.
by a well-known strengthening mechanism: fine grain
strengthening [19,20]. However, the conventional HallePetch
relationship does not apply to SSFSWed joints and requires 2. Materials and methods
further optimizing to explore the softening behavior deeply
[21,22]. 2195-T8 AleLi alloy, a heat-treatable strengthened AleLieCu
So far, previous research has revealed that SSFSW pro- alloy, was rolled and cut into sheets with dimensions of
vides more advantages than CFSW in terms of microstruc- 300 mm  100 mm  12 mm. The chemical composition and
ture and mechanical properties. Contrast tests on 4 mm mechanical properties are shown in Tables 1 and 2. According
6061-T6 sheets confirmed that SSFSW reduced stress con- to Fig. 1a, SSFSW tests were performed on FSW-RL31-016
centrations in the weld and improved tensile properties by along perpendicular to the rolling direction (RD) under a
15.1% over CFSW [23]. Similarly, welding tests on the 5 mm rotational speed of 400 rpm and a welding speed of 60 mm/
3010 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4

Table 1 e Chemical compositions of 2195-T8 AleLi alloy 3. Results


(wt%).
Alloy Cu Fe Mg Zr Li Si Al 3.1. Microstructure features in different regions of
2195-T8 4.04 0.04 0.47 0.11 1.06 0.03 Bal. SSFSWed joints

3.1.1. Grain characteristics and recrystallization mechanisms


min. The stir tool is made up of two components: a stir pin and Figure 2 shows the inverse pole figure (IPF) maps and misori-
a stationary shoulder (Fig. 1c). The stir tool is manufactured of entation angle distributions in different areas of SSFSWed
H13 steel and has a shape referenced to the M10 threaded joint. A black line represents high angle grain boundaries
conical table, where the top diameter is 6.33 mm, the root (HAGBs) with misorientation angles over 15 , while a white
diameter is 11 mm, and the length is 12 mm. line signifies low angle grain boundaries (LAGBs) with orien-
Transmission electron microscopy (TEM), X-ray diffraction tation angles between 2 and 15 . The labeling colors for
(XRD), and electron backscatter diffraction microscopy (EBSD) different grains are based on the IPF coloring system (bottom
were employed to quantify the microstructure evolution in left in Fig. 2) to identify the crystal growth orientation. Figure 3
different areas of the joint, as shown in Fig. 1d. Before carrying shows the recrystallized fraction (RF) maps and histograms in
out TEM tests on an FEI Talos F200X equipped with an energy various regions of the SSFSWed joint, where the blue, yellow
dispersive spectroscopy (EDS), the specimens were prepared and red grains represent recrystallized, substructured and
on a Gatan 691 Ion Beam Thinner. In order to investigate pre- deformed grains.
cipitate evolution in various areas of the whole joint, the bright BM is characterized by a non-homogeneous rolling grain
field (BF) images and selected area electron diffraction (SAED) mainly orientated along <101>//TD. The fraction of LAGBs is
were captured at an accelerating voltage of 200 kV. XRD tests about 44.7%, as shown in Fig. 2a. The fractions of recrystal-
were carried out on a D8 Advanced diffractometer equipped lized, substructured and deformed grains in BM are approxi-
with a Cu target at a Bragg angle of 20 e90 (2q). The acceler- mately 23.37%, 43.59% and 33.04%, respectively, as shown in
ating voltage and current were 40 kV and 40 mA, respectively. Fig. 3a. It reveals that BM has a higher dislocation density
The scan step and speed were 0.02 and 3 /min. The EBSD (Fig. 11d) due to more deformed grains and a lower recrys-
specimens with dimensions of 40 mm  10 mm  12 mm were tallization degree. Subjected only to the welding thermal
cut from the as-welded joints along the weld cross-section, as cycling, HAZ still retains rolling grain characteristics similar
shown in Fig. 1b. A scanning electron microscope (SEM, JSM to BM. One part of crystals in HAZ still remains growing along
7900 F-SEM) with an EDAX-TSL system was utilized for EBSD <101>//TD, while the other part changes to <0.5 0.5 1>//TD.
tests, and TSL OIM software was employed for data processing. The frictional heat in HAZ converts certain rolling grains into
Tensile fracture morphology was analyzed by tungsten fila- equiaxed grains, increasing the fraction of HAGBs to 49.6%
ment scanning electron microscopy (su1510). (Fig. 2b). Due to static recovery and recrystallization in HAZ,
In order to discuss mechanical properties of the whole the fraction of deformed grains drops to 25.12%, whereas
joint, tensile specimens were designed and fabricated, with there is a significant increase in the proportion of sub-
the sampling location and dimension shown in Fig. 1b and d. structured grains to 53.76%. As shown in Fig. 2c, at the
Tensile specimens in different regions were designed and interface between HAZ and TMAZ on the advancing side (AS-
processed to evaluate the variation of mechanical properties HAZ-TMAZ), the area close to HAZ still maintains the primi-
in the joint. The sampling locations and dimensions are tive grain characteristics. Subjected to weaker thermal-
shown in Fig. 1b and d for the yellow and purple specimens, mechanical coupling, grains close to TMAZ tend to bend
respectively. The dimensions of tensile specimens were with an orientation switch to <0.5 0.5 1>//TD under the shear
designed according to ASTM E8/E8M-2016a guidelines. A CSS- friction of the stir pin. The fraction of HAGBs in AS-HAZ-
44100 electronic testing machine was employed to conduct TMAZ increases to 51.0%. Fig. 3c illustrates the increasing
tensile tests in the whole joint at a loading rate of 3 mm/min, degree of recrystallization in AS-HAZ-TMAZ, where the pro-
while an INSTRON 2710-004 instrument was utilized to portion of recrystallized grains climbs to 23.98%. However, a
conduct tensile tests in different areas at a tensile speed of part of substructured grains is transformed into deformed
0.3 mm/min at room temperature. An electronic hardness grains due to shear deformation, bringing the fraction of
tester (HVS-100) was applied to conduct hardness tests on the substructured grains down to 46.2% and the fraction of
cross-section with a load of 300 g for 10 s, where the interval deformed grains up to 29.82%. As shown in Figs. 2 and 3c,
between adjacent hardness spots was 0.5 mm. numerous sub-grain boundaries occur in rolling grains due to
the slip and climb of dislocations, and transform into
recrystallized grains with the increase in misorientation
Table 2 e Tensile properties of 2195-T8 AleLi alloy at angle. The flattened grains are then separated into several
room temperature. smaller grains after being compressed to subcrystalline
Alloy Rolling direction UTS (MPa) YS (MPa) EL (%) thickness. Furthermore, there are a few recrystallized grains
2195-T8 ⊥ 530.5 492.5 7.0 present at grain boundaries. Therefore, the recrystallization
k 546.8 514.1 4.7 mechanisms in AS-HAZ-TMAZ are GDRX, CDRX and DDRX
[31]. Due of the more severe thermal-mechanical coupling,
Note: UTS: ultimate tensile strength; YS: yield strength; EL:
elongation. the long-rolling grains in TMAZ show significant bending
deformation, with an inclination angle around 55 . The
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4 3011

Fig. 1 e Schematic illustration of (a) SSFSW process, (b) sampling positions, (c) stir tool, and (d) dimensions of tensile
specimens.

crystal orientation evolves to <101>//TD under the shearing reduced to 15.21% and 7.75%. It suggests that WNZ has
effect of the stir pin. Nevertheless, the fraction of HAGBs is experienced a higher level of dynamic recrystallization. The
significantly reduced to 36.9%. Combined with RF (Fig. 3d), distribution of large recrystallized grains near grain boundary
TMAZ exhibits a higher fraction (38.19%) of deformed grains crossings is characterized by DDRX, whereas the “necklace”
than AS-HAZ-TMAZ, whereas recrystallized and sub- distribution of plentiful recrystallized grains suggests that
structured grains drop to 18.84% and 42.97%, respectively. It is CDRX is the primary recrystallization mechanism in WNZ
mainly attributed to the shear deformation of recrystallized [34].
and substructured grains by the stir pin. As shown in Fig. 2d, In conclusion, HAZ is primarily where static recovery and
the bent rolling grains display typical GDRX features in that recrystallization occur. The recrystallization mechanisms in
they are continuously extruded and divided [31]. There are AS-HAZ-TMAZ and TMAZ consist mainly of DDRX, CDRX and
smaller recrystallized grains and substantial sub-grain GDRX, while WNZ is dominated by CDRX and DDRX. As a
boundaries in rolling grains, along with a few recrystallized result, the grain features of SSFSW joints show a significant
grains scattered along the grain boundaries, which indicates non-homogeneity under the effects of different temperature
that TMAZ experiences CDRX and DDRX [31]. Exposed to the histories and plastic deformation degrees, namely a gradual
most violent temperature history and plastic deformation, transition from the layered rolling grains in BM to the equi-
WNZ experiences severe dynamic recrystallization, gener- axed grains in WNZ. Except for TMAZ, the fractions of HAGBs
ating equiaxed grains completely replacing rolling grains. and recrystallization degree gradually increase from BM to
However, grain size is significantly smaller towards the bot- WNZ.
tom of WNZ (Fig. 2f) than at the top (Fig. 2e). There is no
obvious crystal preferred orientation at the top of WNZ, 3.1.2. Texture development
whereas grains at the bottom develop mainly along <001>// Fig. 4 shows orientation distribution functions (ODFs) in
TD. Due to slightly higher temperature and plastic deforma- different regions of SSFSWed joint and the fractions of main
tion at the top by cone angle (11 ) of the stir pin, there is a textures. Compared with ideal texture components (Fig. 4g),
higher fraction of HAGBs at the top (76.8%) than at the bottom BM (Fig. 2a) and HAZ (Fig. 2b) possess nearly similar texture
(66.6%). The fraction of recrystallized grains reaches 76.57% types, consisting mainly of stronger rolling textures, Brass
and 87.88% at the top and bottom, respectively, as illustrated {110}<211>, Copper {112}<111>, S {123}<634>, and weaker
in Fig. 3e and f. Deformed grains are decreased to 8.22% and recrystallization textures, Cube {001}<100>, CubeND {001}
4.38% at the top and bottom, while substructured grains are <310>. The intensities in BM and HAZ for rolling crystal
3012 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4

Fig. 2 e IPF maps and misorientation angle distribution in different regions of SSFSWed joint: (a) BM, (b) HAZ, (c) AS-HAZ-
TMAZ, (d) TMAZ, (e) the top of WNZ, (f) the bottom of WNZ.

orientations are up to 16.64 and 22.14, respectively. Rolling orientations under shear stress, sacrificing part of recrystalli-
texture fractions in BM and HAZ reach up to 71.4% (Fig. 4h) zation texture Cube, F and shear texture A to regenerate higher
and 83.4% (Fig. 4i), whereas recrystallization texture frac- proportions of S (22.9%) and Brass (13.3%), as shown in Fig. 4d
tions are only 19.1% and 5.6%, indicating that BM and HAZ and k, leading to an increase in texture intensity to 11.03.
have strong rolling crystal orientations with lower recrys- During the severe plastic deformation of WNZ, recrystalliza-
tallization degrees. In AS-HAZ-TMAZ, exposed to weaker tion nucleation occurs in the deformation zones and develops
shearing by the stir pin, the region near TMAZ produces up to around the large particle, commonly referred to as particle
24.2% of shear texture A {112}<110> (Fig. 4h and j), while the stimulated nucleation (PSN). PSN typically leads to the devel-
higher heat cycle also enhances recrystallization degree. It opment of recrystallization textures [32]. The top of WNZ
increases Cube fraction to 4% and generates up to 6.5% of F {111} (Fig. 4e and l) is mainly composed of various recrystallization
<112>. Moreover, the texture intensity drops to 9.49 with the textures such as F, Goss{110}<100>, CubeND, U{258}<121>, Q
rolling crystal orientation divided by the recrystallization {013}<231>, R{124}<211> and shear textures A, B/ B {111}<110>,
crystal orientation. TMAZ produces flow-deformed preferred Rt Cube{001}<110>, with recrystallization textures and shear
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4 3013

Fig. 3 e RF maps and histograms in different regions of SSFSWed joint: (a) BM, (b) HAZ, (c) AS-HAZ-TMAZ, (d) TMAZ, (e) the
top of WNZ, (f) the bottom of WNZ.

textures accounting for 39.7% and 13.3%, respectively. again. WNZ consists mainly of diverse recrystallization tex-
Recrystallization textures at the bottom of WNZ (Fig. 4f and m), tures and a limited amount of shear textures.
such as U, R, Cube, and F, account for 26.9% compared to 9.4%
for shear texture A. The equiaxed grains completely replace the 3.1.3. Precipitate distribution
rolling grains, disrupting the initial growth direction and Fig. 5 shows TEM images in different regions of SSFSWed joint.
significantly reducing the texture intensity of WNZ to As shown in Fig. 5a, BM is composed of diffusely distributed
3.67e6.85. needle-like precipitates with a length of 60e80 nm and a
In summary, BM and HAZ are primarily dominated by thickness of 3e7 nm. There are distinct diffraction spots at 1/
rolling textures, while AS-HAZ-TMAZ develops shear texture 3<220> and 2/3<220> and diffraction streaks along <111> di-
under the weaker shear stress. Owing to the significant flow rection, as shown in Fig. 5b. The four variants originate from
deformation of the crystals, TMAZ generates rolling textures the superlattice reflection of T1 (Al2CuLi) in BM [33]. There are
3014 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4

Fig. 4 e ODFs in different sections of SSFSWed joint: (a) BM, (b) HAZ, (c) AS-HAZ-TMAZ, (d) TMAZ, (e) the top of WNZ, (f) the
bottom of WNZ, (g) ideal texture components, and the fractions of main textures: (h) BM, (i) HAZ, (j) AS-HAZ-TMAZ, (k) TMAZ,
(l) the top of WNZ, (m) the bottom of WNZ.

a number of coarsened needle-like precipitates that are spherical precipitates (Fig. 5c) are also observed. Therefore, a
densely cross-distributed in HAZ, as shown in Fig. 5c. As a significant quantity of T1/q0 is coarsened in HAZ, along with a
result of the diffused solute atoms by the welding heat cycle, negligible amount of d'/b0 re-precipitating. Compared to HAZ,
the thickness and length of precipitates in HAZ are coarsened the length of T1/q0 is reduced to 30e130 nm in TMAZ, as shown
to 65e160 nm and 5e12 nm, respectively. In addition to T1, a in Fig. 5e, which indicates that needle-like precipitates grad-
tiny quantity of q' (Al2Cu) is also detected, which is determined ually begin to dissolve locally along the edge of lengthwise
by the cross-distributed needle-like precipitates morphology sides. However, it is clear that the thickness of T1/q0 increases
along three directions and the weaker diffraction spots significantly to 12e25 nm, approximately twice as thick as
marked by red circles in Fig. 5d. Furthermore, weaker that in HAZ. Furthermore, amongst the coarsened T1/q0 , there
diffraction spots of d' (Al3Li)/b' (Al3Zr) at 1/2<002>, marked by are dispersed fine spherical precipitates. As shown in the
blue circles in Fig. 5d, as well as a small number of small-sized SAED pattern along [100]Al zone axis (Fig. 5f), it can be
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4 3015

Fig. 5 e TEM images in different regions of SSFSWed joint: (a) the BF image of BM, (b) SAED pattern of BM along [110]Al zone
axis, (c) the BF image of HAZ, (d) SAED pattern of HAZ along [100]Al zone axis, (e) the BF image of TMAZ, (f) SAED pattern of
TMAZ along [100]Al zone axis.

observed that besides the diffraction spots of T1 and q0 , there precipitates with a diameter of around 56 nm are detected
are distinct diffraction spots at 1/2<220> and 1/2<002>, iden- along grain boundaries, while spherical precipitates with a
tified as d'/b' [33]. It can be inferred from the diffraction peaks diameter of about 20 nm are dispersed outside PFZs. EDS
in Fig. 11b that a small amount of T2 is also present in TMAZ. analysis is performed on the precipitates in Fig. 6b in order to
Therefore, TMAZ consists mainly of further coarsened T1/q0 , identify such two precipitates, with results shown in
as well as a few T2 and d'/b'. Fig. 6ced. Since Li cannot be recognized, the precipitate types
Precipitate-free zones (PFZs) with a width of approximately can be identified by the atomic ratios of Al and Cu. The small-
177e236 nm are detected along grain boundaries in AS-HAZ- sized precipitates outside PFZs have an exceptionally low Cu
TMAZ, as shown in Fig. 6aeb. Within PFZs, spherical concentration, referred to as d'. In contrast, the precipitates
3016 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4

Fig. 6 e TEM analysis of AS-HAZ-TMAZ: (a)e(b) the BF images, (c)e(d) EDS spectrums.

within PFZs have an atomic ratio (Al to Cu) of 7.5, identified as According to the EDS spectrum in Fig. 7i, the precipitate has an
T2 (Al6CuLi3). Moreover, the diffraction peak of TB (Al7Cu4Li) is Al/Cu ratio of around 2.3, significantly higher than T2 and
also evident in AS-HAZ-TMAZ, as shown in Fig. 11b. There- equivalent to the atomic ratio in TB. Although TB and T2 share
fore, as result of higher thermal cycling and weaker shear nearly similar dimensions and morphology, there is a clear
deformation, T1/q0 along grain boundaries in AS-HAZ-TMAZ indentation in the transition zone between TB and Al matrix,
dissolves, and cannot re-precipitate in time during cooling, as shown in Fig. 7i. The diffraction peaks shown in Fig. 11b
delivering solute atoms for TB, T2, and d'. indicate that T2 is widely distributed throughout WNZ, while
When combined with Fig. 7a, d and the diffraction peaks TB is more present toward the bottom.
marked in Fig. 11b, it can be observed that the precipitate In summary, BM consists mainly of abundant fine needle-
morphologies at the bottom and top of WNZ are almost like T1. The length and thickness of T1/q0 are coarsened in
identical, consisting of spherical and rod-like precipitates HAZ, as well as a few d'/b0 re-precipitated. Along with the re-
with sizes of 80e180 nm, while needle-like T1/q0 is almost precipitation of TB in AS-HAZ-TMAZ, T1/q0 at the grain
completely dissolved. The top of WNZ is exposed to more boundaries dissolves, forming PFZs and T2 along the grain
severe plastic deformation and higher heat input due to the boundaries. The length of T1/q0 shortens a little bit, thickens
cone angle (about 11 ) of the stir pin, which causes a decrease twice, and a few T2 and d'/b0 are produced in TMAZ. T2 is
in size and gradual dissolution of the precipitates. Conse- scattered throughout WNZ, while TB is mainly detected at the
quently, the density and size of the precipitates at the bottom bottom. Furthermore, the precipitate density is higher at the
are slightly higher than at the top. In order to identify the bottom than at the top.
precipitate types, EDS spectrums are performed on pre-
cipitates in Fig. 7a. According to EDS spectrums in Fig. 7bec 3.2. Mechanical properties in different regions of
and f-h, Al/Cu is approximately 5e6, identified as T2 (Al6CuLi3). SSFSWed joint
It is the first time that significant amounts of T2 have been
discovered to re-precipitate in solid-state welding AleLi alloy 3.2.1. Hardness distribution
joints. The superlattice reflection along <100> direction is The 2D hardness contour map in the thick-plate 2195-T8 AleLi
considered to be TB (Al7Cu4Li) [34], as shown in Fig. 7e. alloy SSFSWed joint is compared with macroscopic
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4 3017

Fig. 7 e TEM images of the whole WNZ: (a) the BF image at the top, (b)e(c) EDS spectrums at the top, (d) the BF image at the
bottom, (e) SAED pattern at the bottom along [100]Al zone axis, (f)e(i) EDS spectrums at the bottom.
3018 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4

Fig. 8 e Hardness distribution of SSFSWed joint: (a) the 2D hardness contour map along ND-RD section, (b) hardness profile
at the top, middle and bottom of the joint, (c) hardness distribution of WNZ along plate thickness.

morphology, as shown in Fig. 8. It can be observed that BM has surface, the hardness values are homogeneously distributed,
the highest hardness value, approximately 160e170 HV. In approximately 120 HV, whereas the hardness values abruptly
HAZ, the area close to BM shows higher hardness values, decrease from 120 HV to around 90 HV within 8e12 mm from
around 160 HV, while the region farther from BM exhibits lower the weld surface. In conclusion, AS-HAZ-TMAZ and the bottom
hardness values. When close to AS-HAZ-TMAZ, the hardness
value drops to the minimum, around 95e100 HV. However, the
hardness values gradually recover from approximately 95 HV
to 120 HV in the narrower TMAZ, whereas the hardness values
adjacent to WNZ eventually rebound to around 120 HV. The
hardness values of WNZ remain constant at around 120 HV.
Furthermore, in the weaker part of the joint, i.e., HAZ-TMAZ,
the hardness values on the advancing side (about 95e105 HV)
are lower than on the retreating side (about 110e120 HV).
Therefore, the overall hardness distribution of SSFSWed joint is
approximate “W”. Fig. 8b shows hardness profiles at the top,
middle, and bottom of the joint, originating from Fig. 8a. It is
obvious that hardness profiles at the top and middle are almost
clear “W”, with the most severe softening in AS-HAZ-TMAZ.
However, the hardness distribution at the bottom is approxi-
mate “U”, with the most severe softening at the bottom of WNZ.
The bottom of WNZ, with a hardness value of around 90 HV,
lower than AS-HAZ-TMAZ, is where the whole joint is most
severely softened. Fig. 8c illustrates the hardness distributions Fig. 9 e Engineering stressestrain curves and fracture
of WNZ along plate thickness. Within 8 mm from the weld location of the entire joints.
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4 3019

Fig. 10 e Tensile properties (a) in different regions of SSFSWed joint and (b) along plate thickness of WNZ, engineering
stressestrain curves (c) in different regions of SSFSWed joint and (b) at the top, middle and bottom of WNZ.

of WNZ are the areas with the lowest hardness values for distribution in different regions of the joint is approximate
SSFSW thick-plate 2195-T8 AleLi alloy joint. “W”. Tensile tests along plate thickness are conducted to
evaluate the softening tendency of WNZ, with the results
3.2.2. Tensile properties shown in Fig. 10b and d. It is evident that the average UTS and
Fig. 9 shows the tensile properties and the fracture location of YS values are around 394 MPa and 259 MPa, homogeneously
the whole joints at 400 rpm, 60 mm/min. It can be observed that distributed along plate thickness within 10 mm from the weld
ultimate tensile strength (UTS) of the whole joint is approxi- surface. However, UTS and YS at the bottom of WNZ are
mately 399 MPa, and elongation is around 5.64%. The crack reduced to 336 MPa and 231 MPa. Along plate thickness, the
extends from the top of AS-HAZ-TMAZ to the bottom of WNZ. elongation increases from 21.4% at the top to 23.9% at the
In order to investigate softening degree in the SSFSWed joint, bottom.
tensile tests in different regions of the joint are carried out, as In conclusion, in the whole SSFSWed joint, the regions
illustrated in Fig. 10a and c. It is noted that BM has the with the lowest tensile strength are the bottom of WNZ and
maximum UTS and yield strength (YS), approximately 530 MPa AS-HAZ-TMAZ, coincident with the crack propagation direc-
and 493 MPa, respectively. In HAZ, UTS and YS gradually tion of the tensile specimen.
decrease from 518 MPa and 478 MPa to 387 MPa and 289 MPa,
with increasing distance from BM, whereas they fall to their
lowest values (370 MPa and 239 MPa) in AS-HAZ-TMAZ, 4. Discussion
respectively. UTS and YS in TMAZ recover gradually from
around 370 MPa, 239 MPa to 392 MPa, 254 MPa, while WNZ 4.1. Softening behavior of SSFSWed joint
generally maintains about 390 MPa and 250 MPa. The elonga-
tion increases monotonically from around 7% in BM to around 2195-T8 AleLi ally, a precipitation-strengthened Al alloy, is
19.3% in WNZ. Although UTS and YS of HAZ-TMAZ on the characterized by four main strengthening mechanisms: solid
advancing side (370 MPa, 239 MPa) are slightly lower than on solution strengthening, fine grain strengthening, precipitation
the retreating side (379 MPa, 246 MPa), they both exhibit a strengthening, and dislocation strengthening [14]. However, it
similar softening tendency in the SSFSWed joint. Conse- is difficult to quantify the variation in solid solution
quently, similar to hardness distribution, tensile properties strengthening in different areas of the joint. The softening
3020 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4

Fig. 11 e The calculation of dislocation density and dislocation increments in different regions of SSFSWed joint: (a) XRD
patterns, (b) the partial enlarged patterns, (c) WilliamsoneHall plots, (d) histograms of dislocation density and dislocation
increments.

behavior in the SSFSWed joints can be explored through where b is the peak width at half-peak height, l is the wave-
dislocation density, precipitate evolution, and the HallePetch length of the X-rays (0.1542 nm for Cu Ka), D is the crystal size,
relationship. ε is the lattice strain, and q is the Bragg angle. After bringing b
and q from the XRD pattern (Fig. 11a) into Eq. (2), b cos
l
q
and 2 sin
l
q

4.1.1. Influence of dislocation density on softening behavior can be calculated by linear fitting, as shown in Fig. 11c ε is the
During SSFSW, different regions in thick-plate AleLi alloy slope of the fitting curve [37]. The dislocation increments and
joint suffer from heterogeneous temperature histories and dislocation density in different areas of the joint can be
plastic deformation. The heterogeneous dislocation density calculated by Eqs. (1) and (3), respectively, with the results
distribution that results from the various recovery and displayed in Fig. 11d.
recrystallization degrees in the SSFSWed joint has a signifi- After rolling and T8 treatment, BM retains high-density
cant impact on the softening behavior. The YS increment of dislocation, with the dislocation density and dislocation
dislocation density can be evaluated by Eq. (1) [35]: increment of around 2.09  1015 m2 and 205.53 MPa, as shown
in Fig. 11d. HAZ experiences recovery and recrystallization
Dsdis ¼ MaGbr1=2 (1)
under the thermal cycle, reducing dislocation density and
where Dsdis is dislocation increment, M is the Taylor factor dislocation increment to 1.10  1015 m2 and 149.42 MPa,
(3.06), a is the geometric factor of Al alloy (0.2), G is the shear respectively. Subjected to the weaker thermo-mechanical
modulus of the aluminum alloy (26.2 GPa), b is the Burgers coupling for dynamic recovery and recrystallization in AS-
vector (0.2864 nm), and r is the dislocation density. The HAZ-TMAZ, the dislocation density and dislocation incre-
dislocation density can be calculated by Eqs. (2) and (3) [18,36]: ment are dramatically reduced to 5.34  1014 m2 and
104.02 MPa. One of the main reasons for the higher softening
b cos q 0:9 2ε sin q degree in AS-HAZ-TMAZ is that the retreating side, with less
¼ þ (2)
l D l
deformation than the advancing side, has a higher dislocation
ε2 density and dislocation increment of 7.38  1014 m2 and
r ¼ 16:1 (3)
b2 122.25 MPa, respectively. Exposed to more intense shear
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4 3021

deformation, the dislocation density and dislocation incre- tension. It improves plasticity and toughness and alleviates
ment on the advancing side of TMAZ increase to the fracture tendency while having an extremely weak effect
7.39  1014 m2 and 122.31 MPa, whereas they are on strength [42]. Furthermore, AS-HAZ-TMAZ is accompanied
4.84  1014 m2 and 98.98 MPa on the retreating side of TMAZ by the re-precipitation of TB, which usually nucleates on Si-
with weaker deformation degree. The violent deformation containing particles in the spherical precipitate b'/d0 ,
and heat input at the top of WNZ release the dislocations, depleting the solute atoms available for forming supersatu-
leading to lower dislocation density and dislocation incre- rated solid solution zones and leading to a reduction in me-
ment at the top (6.50  1014 m2, 114.74 MPa) than at the chanical properties [34]. Due to forming PFZs at grain
bottom (1.19  1015 m2, 155.09 MPa). boundaries and re-precipitating TB, AS-HAZ-TMAZ exhibits
In conclusion, a comparison with the tensile properties less T1/q0 coarsening and more severe softening than TMAZ.
shows that the decrease in dislocation density is the main T1/q0 is completely dissolved in the whole WNZ, with signifi-
reason for the SSFSWed joint softening. However, the soft- cant abundant T2 dispersing, while TB is only re-precipitated
ening behavior of WNZ along plate thickness cannot be at the bottom of WNZ. Therefore, the dissolution of T1/q0 is
reasonably explained in terms of dislocation density. responsible for the softening in the whole WNZ, whereas re-
precipitating TB leads to a higher softening degree at the
4.1.2. Influence of precipitate evolution on softening behavior bottom. The higher elongation at the bottom than the top
The precipitate-strengthened 2195-T8 AleLi alloy has an (Fig. 10d) is attributed to re-precipitating the higher density of
extremely complex precipitate system, and SSFSW involves a T2.
complex thermo-mechanical coupling process, which causes In conclusion, the coarsening and dissolution of T1/q0 , and
coarsening, dissolution, and re-precipitation of precipitates in transformation into b'/d0 , TB and T2 are fundamentally
different regions of SSFSWed joint [16]. The joint softening responsible for the softening in different regions of the
behavior is therefore closely related to precipitate evolution. It SSFSWed joint. The severe softening in AS-HAZ-TMAZ is
is known from previous studies that the dislocation move- mainly caused by forming PFZs along grain boundaries and re-
ment is mainly by bypassing precipitate and leaving a dislo- precipitating TB, while the dissolution of T1/q0 and re-
cation ring. The increment of precipitation strengthening precipitating TB are responsible for the extreme softening at
caused by the bypassing mechanism can be evaluated by Eq. the bottom of WNZ.
(4) [38,39]:
rffiffiffiffiffiffiffiffiffiffi! 4.1.3. Influence of HallePetch relationship on softening
gapb 3p2 f behavior
Dsp;by ¼ 0:81M (4)
2b 8 Fine grain strengthening is also a widely recognized
strengthening method [19,20]. However, the conventional
where Dsp;by is the increment of precipitation strengthening
HallePetch relationship is limited to explaining the relation-
due to the bypassing mechanism, gapb is the antiphase
ship between grain size and YS, ignoring the effect of crystal
boundary energy, f is the volume fraction of the precipitates.
orientation [21,22]. Therefore, an optimized model is pro-
Needle-like T1 and q0 , with higher antiphase boundary en-
posed, as follows [43]:
ergies (gapb ) and the ability to hinder dislocation movement,
are the two most effectively strengthened precipitates in 2195- .
1=2 1=2
Dsy ¼ 3ðptc Gb=2maÞ d m (5)
T8 AleLi alloy [33,40]. It is the fundamental reason for the
highest strength and hardness in BM. Due to the lower weld where Dsy is YS increment of the HallePetch relationship, d is
thermal cycle, T1/q0 coarsens in HAZ and is accompanied by grain size, tc is the critical shear stress of polycrystal, m is
the precipitation of d'/b0 , weakening the strengthening effect. schmid factor, the ratio 3 is from well-accepted Tabor's rela-
A metastable phase d'/b0 , precipitating at lower temperatures tion between indentation hardness and YS of a material, an
with lower activation and interfacial energy, contributes to average dislocation character is expressed in the factor
effective pinning grain boundaries and promoting grain a2 ¼ 2(1y) (2y), y is Poisson's ratio. The optimized HallePetch
refinement. Although d'/b0 also contributes to improving me- relationship primarily describes the relationship among YS,
chanical properties, the strengthening effect is significantly grain size, and schmid factor.
weaker than T1/q0 due to the lower antiphase boundary energy In the SSFSWed joint, rolling grains from BM to WNZ are
(gapb ) [33,40]. T1/q0 in TMAZ is locally dissolved at the long edge continuously divided, refined, and transformed towards
and further coarsened in thickness, weakening the strength- equiaxed grains due to various recrystallization degrees,
ening effect. Higher welding thermal cycling and weaker whereas the strength and hardness are gradually reduced.
shear deformation lead to the dissolution of the precipitates Moreover, the grain size in WNZ also decreases significantly
and migration of Cu atoms at the grain boundaries of AS-HAZ- along plate thickness, but the strength and hardness are
TMAZ. However, it does not have enough time to re- significantly weaker at the bottom than at the top and middle.
precipitate substantially during cooling, contributing to It suggests that grain size does not seems to be a critical factor
forming PFZs and T2 phase along grain boundaries. PFZs lose affecting the YS increment, according to the conventional
the hindrance of precipitates relative to dislocation move- HallePetch relationship. It is known from previous studies [44]
ment, leading to localized softening [41]. The interface be- that the orientation factor plays a significant role in the joint
tween T2 and Al matrix is smooth and flat, and the softening behavior. Compared to other textures, the average
compression effect produced during precipitation inhibits the of the five maximum Schmid factors for eight groups of
nucleation and extension of cracks along the interface during symmetrical slip systems in Cube is up to 0.41. It contributes
3022 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4

to being in a soft orientation during tension and tends to indicated that the softly oriented grains are more abundant at
soften in localized areas. The fraction of Cube increases from the bottom of WNZ and in AS-HAZ-TMAZ, resulting in lower
1.1% in BM to 4% in AS-HAZ-TMAZ, as shown in Fig. 4hej, and YS increments. In conclusion, the softening degrees are
decreases to 3.3% in TMAZ (Fig. 4k). The fraction of Cube is higher at the bottom of WNZ and in AS-HAZ-TMAZ with
much lower at the top of WNZ (1.4%) than at the bottom (13%), higher fractions of the maximum schmid factor (distributed in
as illustrated in Fig. 4lem. Therefore, the fraction distribu- 0.4e0.5) and Cube.
tions of Cube in different regions of the SSFSWed joint are
opposite to the distributions of tensile strength and hardness. 4.2. Fracture modes in different regions of SSFSWed
Furthermore, in a previous study [44], the fractions of the joint
maximum schmid factor (distributed in 0.4e0.5) are signifi-
cantly higher at the bottom of WNZ (96.89%) and in AS-HAZ- Figure 12a shows the fracture morphology of BM. It can be
TMAZ (95.13%) than in other regions of SSFSWed joint. It observed that there are a large number of elongated cracks

Fig. 12 e The fracture morphologies in different regions of SSFSWed joint: (a) BM, (b) HAZ, (c) AS-HAZ-TMAZ, (d) TMAZ on the
advancing side, (e) HAZ-TMAZ on the retreating side, (f) the top of WNZ, (g) the middle of WNZ, (h) the bottom of WNZ.
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 3 0 0 8 e3 0 2 4 3023

distributed at grain boundaries along the rolling direction. homogeneously distributed within 8 mm from the weld
There are also a large number of short, crooked tear ridges and surface but considerably drop within 8e12 mm. The most
smooth quasi-cleavage facets. Moreover, a few dimple bands severely softening regions in the SSFSWed joint are the
are distributed non-homogeneously along the rolling direc- bottom of WNZ and AS-HAZ-TMAZ. The fracture mecha-
tion across the whole fracture morphology. Therefore, the nism transforms from quasi-cleavage fracture in BM to
fracture mode of BM (elongation is about 7%) is concluded to plastic fracture in WNZ.
be a quasi-cleavage fracture, a transitional fracture mode 4. The joint softening is partly attributed to a decline in
between cleavage fracture and dimple fracture. Similar to BM, dislocation density. The coarsening and dissolution of T1/q0
the fracture morphology of HAZ consists of elongated cracks and transformation to d'/b0 , TB and T2 are the primary
along the rolling grain boundaries, dimple bands, and quasi- reason for various softening degrees in the SSFSWed joint.
cleavage facets, typical characteristics of quasi-dissociation The severe softening in AS-HAZ-TMAZ is caused by form-
fracture, as shown in Fig. 12b. The number and depth of ing PFZs and re-precipitating TB, whereas that at the bot-
dimples increase significantly in AS-HAZ-TMAZ, as shown in tom of WNZ is attributed to re-precipitating TB and the
Fig. 12c. The formation of PFZs is primarily responsible for the complete dissolution of T1/q'. AS-HAZ-TMAZ and the bot-
dispersed distribution of small and flat quasi-cleavage facets. tom of WNZ, with higher fractions of the maximum
It indicates that AS-HAZ-TMAZ begins to exhibit a plastic schmid factor (in 0.4e0.5) and Cube texture, tend to be in
fracture feature with elongation increasing to 15.5%. However, soft orientation.
the fracture morphology of HAZ-TMAZ on the retreating side
(Fig. 12e) shows numerous quasi-cleavage facets, dimples, and
Declaration of Competing Interest
tear ridges, confirming the fracture mechanism to be a quasi-
cleavage fracture. The number and size of quasi-cleavage
The authors declare that they have no known competing
facets in TMAZ gradually decrease, accompanied by a scat-
financial interests or personal relationships that could have
tered distribution of small-sized dimples, as shown in Fig. 12d.
appeared to influence the work reported in this paper.
Therefore, TMAZ gradually transforms towards a plastic
fracture mode, with elongation increasing to around 17.0%. As
shown in Fig. 12feh, WNZ consists mainly of large equiaxed Acknowledgements
dimples with particles distributed inside, which exhibits the
typical features of plastic fracture. The elongation of WNZ The authors gratefully acknowledge the sponsorship from The
monotonously rises from 21.4% to 23.9%, with the number and National Natural Science Foundation of China (51775371 and
depth of dimples gradually increasing from top to bottom, 52175356), Tianjin Natural Science Foundation (19JCZDJC39200),
representing the higher plasticity and toughness at the bot- and Tianjin Research Innovation Project for Postgraduate Stu-
tom. In conclusion, the fracture mechanism from BM to WNZ dents (2021YJSO2S05).
gradually changes from quasi-cleavage fracture to plastic
fracture, with the elongation changing from 7% to 23.9%.
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