Materials Science & Engineering A 771 (2020) 138545

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Materials Science & Engineering A

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

Effects of post-weld heat treatment on the microstructure and mechanical

properties of laser-welded NiTi/304SS joint with Ni filler
Yuhua Chen a, *, 1, Songwei Sun a, 1, Timing Zhang a, **, Xingwen Zhou b, Shuhan Li a
a
School of Aerospace Manufacturing Engineering, Nanchang Hangkong University, 696 Fenghe South Road, Nangchang, Jiangxi province, 330063, China
b
School of Mechanical Engineering and Automation, Beihang University, Beijing, 100191, China

A R T I C L E I N F O A B S T R A C T

Keywords: Adding Ni as filler material is one of the effective methods to restrain the cracks in laser-welded joints of NiTi/
Dissimilar metals welding stainless steel (SS), while the formation of Ni3Ti at the NiTi/Ni interface result in uneven distribution of the
Laser welding microstructure of the joint, which limits tensile strength of the joint. In this study, post-weld heat treatment
NiTi shape memory alloy
(PWHT) at 650 � C and 850 � C were applied on a defect-free NiTi/Ni/SS joint to improve its mechanical prop­
Intermetallic compounds
Post-weld heat treatment
erties. As the PWHT temperature increases, more Ni3Ti was observed at the weld metal. This precipitation
strengthened the weld metal, resulting in the average hardness of the weld metal increased from 375 HV0.2 to
493 HV0.2. Owing to the homogenization of microstructure of joints after PWHT, the tensile strength of the joint
improved. The highest joint average strength reached 643 MPa at 850 � C PWHT, which is about 2.12 times higher
than that of the as-welded joint.

1. Introduction
NiTi shape memory alloys (SMAs) are widely used in aerospace,
communication, instrument and medical device fields due to its special
functional characteristics, such as shape memory performance (SME)
and super-elasticity (SE) [1–5]. However, a single NiTi alloy structure
cannot meet the performance requirements of different products.
Therefore, NiTi alloy is often welded to stainless steel (SS) which has
excellent properties to expand its application range [6–9]. For example,
the NiTi/SS guide wire for catheters and dental composite arch wire,
which concentrate the both advantages of NiTi alloy and SS [10–12].
Pulsed laser welding is desirable for welding of NiTi thin sheets,
owing to its advantages of high energy density, deep penetration, nar­
row heat affected zone (HAZ) and minor weld distortion [13–17]. As a
fusion welding technique, NiTi/SS laser welding is challenging due to
the formation of brittle intermetallic compounds (IMCs), such as Ti2Cr,
Ti2Ni, and Fe2Ti [18–20]. These brittle IMCs are usually responsible for
the undesirable mechanical properties of the NiTi/SS joints [21]. One
method for reducing the formation of brittle phases is leading an
interlayer, such as copper [12,22], nickel [11,18,23] and silver-based
filler metal [24]. Among these interlayers, Ni is an optimal filler for
joining of NiTi and SS alloys due to its excellent performances, such as
high corrosion resistance and strength [11,18]. It has been reported that
the tensile strength of laser-welded NiTi/SS joints could be improved by
using Ni as the filler metal, due to the decrease of brittle IMCs (such as
TiFe2 and TiCr2) in the weld metal [18].
Proper post-weld heat treatment (PWHT) on the laser-welded NiTi
joint is an effective method to improve its performance [25,26]. It was
reported that PWHT temperature significantly affects the microstructure
and strength properties of the as-welded NiTi joints due to the formation
of Ni4Ti3, Ni3Ti2, and Ni3Ti IMCs [27–29]. In the case of NiTi/SS joint,
PWHT at 200 � C releases the residual stresses of the joint and slightly
increases the joint strength, while a higher PWHT temperature (400 � C)
results in the formation of brittle IMCs and deteriorates its mechanical
properties [29]. This indicates the PWHT parameter has a significant
influence on the joint’s performance. Therefore, it is necessary to further
study the effect of PWHT temperatures on the microstructure and me­
chanical properties of NiTi/Ni/SS joints, and thus to improve the me­
chanical properties of the joint.
In the present study, PWHT was performed on the laser-welded NiTi/
Ni/304SS joint. The effects of PWHT at different temperatures on the
NiTi/Ni interface, weld metal and base metal of the joint had been

* Corresponding author.
** Corresponding author.
E-mail addresses: ch.yu.hu@163.com (Y. Chen), zhangtm@nchu.edu.cn (T. Zhang).
1
These authors contributed equally to this work.

https://doi.org/10.1016/j.msea.2019.138545
Received 11 September 2019; Received in revised form 10 October 2019; Accepted 11 October 2019
Available online 12 October 2019
0921-5093/© 2019 Elsevier B.V. All rights reserved.
Y. Chen et al.
Table 1
Chemical compositions of base metals (wt. %).
Material Ti Ni C Cr
NiTi 44.34 55.66 – –
SS304 0.54 9.72 0.08 18.07
Fig. 1. Schematic diagram for laser welding of NiTi SMA and stainless steel with Ni filler.
discussed. Its objective is to provide some theoretical basis for improving
the mechanical properties of the NiTi/Ni/304SS joint.
2. Experimental
0.2 mm-thick hot rolled Ti-49.4Ni (at. %, NiTi SMA) shape memory
alloy which were purchased from Beijing GEE Co., Ltd. and AISI304
stainless steel (304 SS) sheet were used as base metals in this investi­
gation. The sheets were prepared to dimensions of 25 mm � 20 mm
using a wire electrode cutting machine. Pure Ni (99 at. %) wires with a
diameter of 0.3 mm were used as filler. Before welding, the oxide layer
on the base metals and filler were removed by grinding, and then ul­
trasonically cleaned in an acetone bath for 15 min, followed by 5 min of
cleaning in distilled water. The chemical compositions of base metals are
listed in Table 1.
Fig. 1 depicts the schematic diagram for laser welding of NiTi SMA
and stainless steel with Ni filler. The optimum laser welding parameters
used in this study were 18.4 W (Laser power), 3.0 Hz (Frequency),
5.1 m s (Pulse width) and 0.3 m min 1 (Welding speed). Welding pro­
cess was performed using a Nd:YAG laser welding system (Type SL80).
In the welding process, the glass protective cover was used for overall
argon protection, and the flow rate of shielding gas was 10 L⋅min 1. Ar
gas was introduced into the lower side of the protective cover for 2 min
before welding to prevent N2, O2, and H2 from penetrating into the weld
zone to avoid deterioration of the joint properties. The laser was applied
to the middle of the filling material and focused on the surface of the
filler. PWHT process was performed using a box resistance furnace (Type
SX2-5-12). PWHT was conducted by annealing the samples at 650 � C
and 850 � C for 3600 s followed by air quenching.
Fig. 2. Tensile properties of the test samples: (a) Tensile strength and elongation of the joints. (b) Typical tensile curves of the joints.
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Materials Science & Engineering A 771 (2020) 138545
Mn Si P S Fe
– – – – –
2.00 1.00 0.04 0.05 Bal.
For metallographic studies, the specimens were cold mounted by
epoxy and then ground by sand papers from 800 to 3000 SiC grades,
followed by polishing with diamond grinding paste. Laser-welded joint
specimens were etched with an acid solution containing HF:HNO3:H2O
(1:4:5) for 13–18 s. The chemical compositions, microstructure and
fracture surface morphology of the joints were examined using optical
microscopy (MR5000 Inverted Metallographic Microscope) and scan­
ning electron microscopy (SEM Mode NOVA NANOSEM 450) equipped
with energy-dispersive spectroscopy (EDS). A Rigaku Rapid IIR was used
for XRD analysis and the parameters were set at 40 kV and 250 mA using
Cu Kα radiation.
All mechanical property tests were conducted at room temperature.
A series of hardness values were measured along the longitudinal
centerline of the weld zone and the base metal using Qness Q10A þ fully
automatic hardness testing system at a load of 200 gf and a dwell time of
10 s. Instron 5543 precision tensile test machine was used to measure
the strength and elongation of the joints. The tensile specimens of the
joints and NiTi base metal were machined to a size of 40 mm � 3 mm �
0.2 mm, with a gauge length of 30 mm, and the displacement velocity of
tensile specimen was 0.4 mm/min. Three samples for the joints at
different states and NiTi base metal were tested. Tensile strength and
elongation up to fracture average values were obtained. The fracture
surfaces were examined by SEM and EDS.
3. Results and discussion
3.1. Mechanical properties
Fig. 2 presents the tensile properties of the joints and NiTi base
Y. Chen et al.
Fig. 3. Typical cross-section of the NiTi/Ni/SS joints: (a) As-welded, (b) PWHT at 650 � C, (c) PWHT at 850 � C.
Fig. 4. The microstructure at the NiTi/Ni interface of the joints: (a) As-welded, (b) PWHT at 650 � C, (c) PWHT at 850 � C, (a1~c1) are the enlarged views in (a~c).
metal. The average tensile strength and elongation to fracture of the NiTi
base metal are about 822 MPa and 33%, respectively. The average ten­
sile strength of as-welded joints is approximately 303 MPa. When the
PWHT temperature is increased to 650 � C, the tensile strength increases
to approximately 384 MPa. PWHT at 850 � C joint exhibits the highest
average tensile strength and elongation, which are about 643 MPa and
12% respectively, which are 2.12 and 3.91 times higher than that of the
as-welded joints, respectively. This reflects a trend of increasing average
tensile strength and elongation of the joint with the increase in PWHT
temperature. In addition, the stress-strain curve of PWHT at 650 � C joint
shows obvious yield plateau (see Fig. 2b). These phenomena may be
caused by the difference in the microstructures of the joints.
3.2. Microstructure
To reveal the performance improvement mechanism, the
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Materials Science & Engineering A 771 (2020) 138545
microstructure analysis was performed. Fig. 3 shows the typical cross-
section morphology of defect-free NiTi/Ni/SS joint at different states,
in which the weld metal, heat affected zone (HAZ) and base metal (BM)
are labeled. In our study, PWHT had no significant influence on the joint
morphology. The PWHT at 850 � C joint showed a slight oxide layer,
however the oxide layer had little effect on the mechanical properties of
the joint. As seen in Fig. 3, a inhomogeneous interfacial zone, usually the
weak zone of the joints [18,20], was observed next to the NiTi BM
(NiTi/Ni interface). Besides, an obvious boundary with a small interfa­
cial (Ni/SS interface) at the weld root was observed at the stainless steel
side.
Fig. 4 presents the microstructure of the NiTi/Ni interface of the as-
welded joint and PWHT joints. The NiTi/Ni interface of the as-welded
joint can be divided into two layers (see Fig. 4a1), in which the thick­
ness of the one next to the NiTi BM gradually decreased as the PWHT
temperature increases. The EDS results of these layers are listed in
Y. Chen et al. Materials Science & Engineering A 771 (2020) 138545

Table 2 observed at the weld metal after PWHT. The peaks strength of Ni3Ti at
EDS analysis results of the NiTi/Ni interface marked in Fig. 4 850 � C PWHT was significantly higher than that at 650 � C PWHT, indi­
Point Chemical compositions (at. %) Possible phase cating the increase of Ni3Ti content. Fig. 5b–d presents the microstruc­
ture morphologies of the weld metal at different states. As seen, some
Ti Ni Fe Cr
fine precipitates were observed at the weld metal of the PWHT at 650 � C
A 38.77 59.21 2.01 – NiTi þ Ni3Ti joint. These particles were compounds of Ni3Ti (Ni–58.81 Ti–17.07
B 25.42 68.15 5.34 1.09 Ni3Ti
C 49.87 50.13 – – Ni4Ti3
Fe–18.27 Cr–3.65 Mn–2.19, at.%). Similar to we mentioned above, the
D 27.60 67.78 4.62 Ni3Ti filler Ni wire effectively isolates the reaction of Ti, Fe and Cr elements to
form brittle IMCs during welding. The as-welded weld metal contains
almost no Ti element. In the PWHT process, Ti element diffuses from the
Table 2 to identify their compositions. Combined with the morphology NiTi/Ni interface to the weld metal. The diffusion coefficient of Ti
analysis, the layer close to the NiTi BM is mainly eutectic structure of element is higher than that of Ni element (Diffusion coefficient Ti:
NiTi and Ni3Ti via the EDS result. According to the Ni–Ti phase diagram 1.5 � 10 12 cm2 s 1 and Ni: 2.0 � 10 10 cm2 s 1 at 1223 K [34]), and the
[30], the layer close to the weld metal is mainly Ni3Ti IMCs [11,18,30]. atomic ratio of Ni and Ti in the weld metal is more than 3, thus Ni3Ti is
This indicates that the Ni3Ti content increases as the PWHT temperature formed in the weld metal. In addition, the diffusion coefficient of Ti
increases. During the PWHT process, increasing of the temperature element increases with the increase of the PWHT temperature [35], thus
would increase the diffusion coefficient [25,26], thereby promoting promoting the growth of Ni3Ti in the weld metal.
inter diffusion at the interface. This results in the enhancement of the Ni Fig. 6a shows the microstructure of the Ni/SS interface of the as-
element dilution at this eutectic structure due to its higher concentra­ welded joints. The interfacial zone at this side consists of refined
tion. Therefore, when PWHT temperature increased to 850 � C, this columnar dendrite with a preferential orientation towards the weld
interface was all Ni3Ti IMCs (Fig. 4c1). center. Fig. 6b depicts the EDS line scanning result along the “scanning
Notably, some gray precipitates, maybe the Ni4Ti3 characterized via line” in Fig. 6a. The EDS result shows that the content of elements in this
the EDS result, were observed at the HAZ next to NiTi BM (Fig. 4b). After interfacial zone is close to the 304SS BM, suggesting this region is mainly
PWHT at 850 � C, these precipitates disappeared (Fig. 4c). The Ni4Ti3 consists of the re-solidified 304SS BM. Macro-segregation results in the
phase is an intermediate phase between the NiTi phase and the Ni3Ti formation of this interfacial zone, as reported by T. Soysal et al. [36].
phase, resulting in the variation of the precipitate. As the aging tem­ During PWHT process, no new phases were observed in our joints (see
perature increases, Ni4Ti3 phase transforms into the Ni3Ti equilibrium Fig. 6c and d). This interface is not the weak zone of the joint [18,20], so
phase, which is consistent with Otsuka’s results [30]. These Ni4Ti3 has a we will not discuss the evolution of this interface in detail.
significantly influence on the performance of NiTi base metal [30–33].
As mentioned above, the tensile strength and elongation of the joints
were improved after PWHT at 650 � C, which may be caused by the 3.3. Micro-hardness
precipitation of Ni4Ti3 phase [31].
Fig. 5a shows the XRD patterns of the weld metal at various states. The micro-hardness profiles of the joints are shown in Fig. 7. The
The weld metal without PWHT only consisted of Ni-rich solid solution micro-hardness value of all the joints reach the maximum at the NiTi/Ni
(PDF#47-1417), while the peaks of Ni3Ti (PDF#65-2038) were interface, which is mainly attributed to the highest content of the Ni3Ti

Fig. 5. (a) XRD patterns of the weld metal at different states. The microstructure of the weld metal of the joints: (b) As-welded, (c) PWHT at 650 � C, (d) PWHT at
850 � C. Insets are the enlarged views in (b ~ d).

4
Y. Chen et al.
Fig. 6. The microstructure of the Ni/SS interface of the joints: (a) As-welded, (b) Results of scanning line test in (a), (c) PWHT at 650 � C, (d) PWHT at 850 � C. The
crack-like in (c and d) is because of excessive corrosion in the Ni/SS interface.
Fig. 7. Micro-hardness profiles of the joints. Inset is cross-sectional of NiTi/Ni/
304SS joint. White line indicates the hardness test position.
[5,10]. As the Ni3Ti content increases at this interface, the maximum
hardness value increases as the PWHT temperature increases. The
average micro-hardness of the weld metal without PWHT is about 375
HV0.2, and then it increases to about 440 HV0.2 at 650 � C PWHT, and
further increases to 493 HV0.2 at 850 � C PWHT. This is because of the
increased Ni3Ti in the weld metal. Notably, the difference between the
maximum hardness value and the average hardness of the weld metal is
gradually reduced as the PWHT temperature increases (as-welded ¼ 87;
PWHT at 650 � C ¼ 70; PWHT at 850 � C ¼ 57). These results indicate that
the microstructure of joint gradually homogenizes as the PWHT tem­
perature increases. The minimum micro-hardness values are observed at
the PWHT at 650 � C NiTi HAZ. This may be caused by precipitation of
Ni4Ti3 phase and grain coarsening. Similarly, the hardness of PWHT at
850 � C Ni/304SS interface and 304SS HAZ is much lower than that of
other joints. The grain size at this interface and HAZ of the PWHT at
850 � C joint is coarser than that of other joints, so the hardness at this
5
Materials Science & Engineering A 771 (2020) 138545
interface and HAZ is lower than that of other joints, which conforms to
the Hall-Petch relationship [37]. The micro-hardness distribution of the
joints is consistent with previous research results [26,29].
3.4. Fracture analysis
To understand the mechanisms involved, the fracture surfaces
analysis was performed. The fracture surface and fracture path of
different states joints are shown in Fig. 8. Fig. 8a shows the fracture
morphology of the as-welded joint, which displays the corresponding
fracture surface with a typical brittle fracture. The results of EDS anal­
ysis show that the Ni/Ti atom ratio in the bright feature is approximately
3:1 (Table 3). Cracks propagated along NiTi/Ni interface (see Fig. 8a
inset). A large amount of Ni3Ti at this interface result in uneven distri­
bution of the microstructure of the joint, which limited the tensile
properties of the joint.
After PWHT at 650 � C, the fracture surface was consisted of Ni3Ti and
NiTi via the EDS result of point F and G (Table 3). The fracture path of
PWHT at 650 � C joint is shown in Fig. 8b inset. As seen the crack was first
initiated at NiTi/Ni interface, and a transgranular fracture mode was
observed in this part. The final rupture occurred in the NiTi HAZ, this
part showed a typical ductile fracture. The improvement on the ductility
(Fig. 2b) result from the precipitation of Ni4Ti3 in NiTi HAZ after PWHT
at 650 � C. The precipitation of Ni4Ti3 increases the critical stress for slip
of NiTi alloy, which improves the superelastic properties of NiTi alloy
[30]. And the yield plateau is one of the characteristics of good super­
elasticity, so the tensile curve of the PWHT at 650 � C joint shows obvious
yield plateau.
Similarly, the fracture surface of PWHT at 850 � C joint was almost
entirely NiTi via the EDS result of point H (Table 3). This fracture path
was significantly different from other joints. As seen in Fig. 8c inset,
NiTi/Ni interface was not weak zone of the joint and the crack propa­
gated along NiTi BM. This part exhibited a brittle rupture visible by the
succession of flat surfaces with steps in between. As noted above, NiTi/
Y. Chen et al. Materials Science & Engineering A 771 (2020) 138545

Fig. 8. The fracture surface of the joints: (a) As-welded, (b) PWHT at 650 � C, (c) PWHT at 850 � C. Insets illustrate the fracture path of the joints.

Data availability
Table 3
EDS analysis results marked in Fig. 8 The data used to support the findings of this study are available from
Point Chemical compositions (at. %) the corresponding author upon request.
Ti Ni Fe Cr
Declaration of competing interest
E 22.92 65.54 9.51 2.03
F 36.90 58.37 3.97 0.76
G 50.78 49.22 – – The authors declare that they have no known competing financial
H 49.75 50.25 – – interests or personal relationships that could have appeared to influence
the work reported in this paper.

Ni interface was all Ni3Ti and a large amount of Ni3Ti precipitated in the
Acknowledgments
weld metal after PWHT at 850 � C, which indicate that the microstruc­
ture of the joints homogenized. Owing to this homogenization of
The research was financially supported by National Natural Science
microstructure at the joints, the tensile strength is improved.
Foundation of China (No. 51565040), the Fund for Jiangxi Distin­
guished Young Scholars (2018ACB21016), the project for Jiangxi ad­
4. Conclusions
vantageous scientific and technological innovation team
(20171BCB24007), and Frontier Science Research Project of Educa­
In this study, effects of PWHT on microstructures and mechanical
tional Commission of Jiangxi Province (KJLD14055).
properties of NiTi/Ni/304SS joint were investigated, and the following
conclusions were obtained:
References

(1) A growing number of Ni3Ti IMCs were precipitated at the NiTi/Ni
interface and the weld metal with the increase in PWHT tem­
perature. After PWHT at 650 � C, Ni4Ti3 phase was precipitated at
NiTi BM.
(2) The PWHT at 850 � C weld metal exhibited the highest average
micro-hardness value of 493 HV0.2. The precipitation of Ni3Ti
IMCs in the weld metal is the reason for this variation. The
microstructure of the joints gradually homogenized as the PWHT
temperature increases.
(3) After PWHT at 850 � C, the average tensile strength and elonga­
tion of the joint reached 643 MPa and 12% respectively, which
were 2.12 and 3.91 times higher than that of the as-welded joint.
Homogenization of microstructure at the joint is responsible for
this improvement.
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