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Cryogenics 83 (2017) 1–7

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Cryogenics
journal homepage: www.elsevier.com/locate/cryogenics

Research paper

Effect of post weld heat treatment on the microstructure and mechanical


properties of ITER-grade 316LN austenitic stainless steel weldments
Jijun Xin a,b, Chao Fang a,⇑, Yuntao Song a, Jing Wei a, Shen Xu a, Jiefeng Wu a
a
Institute of Plasma Physics, Chinese Academy of Sciences, Hefei 230031, China
b
University of Science and Technology of China, Hefei 230026, China

a r t i c l e i n f o a b s t r a c t

Article history: The effect of postweld heat treatment (PWHT) on the microstructure and mechanical properties of ITER-
Received 8 November 2016 grade 316LN austenitic stainless steel joints with ER316LMn filler material was investigated. PWHT aging
Received in revised form 29 December 2016 was performed for 1 h at four different temperatures of 600 °C, 760 °C, 870 °C and 920 °C, respectively.
Accepted 2 February 2017
The microstructure revealed the sigma phase precipitation occurred in the weld metals heat-treated at
Available online 4 February 2017
the temperature of 870 °C and 920 °C. The PWHT temperatures have the less effect on the tensile
strength, and the maximum tensile strength of the joints is about 630 MPa, reaching the 95% of the base
Keywords:
metal, whereas the elongation is enhanced with the rise of PWHT temperatures. Meanwhile, the sigma
316LN austenitic stainless steel
Post weld heat treatment
phase precipitation in the weld metals reduces the impact toughness.
Impact toughness Ó 2017 Elsevier Ltd. All rights reserved.
Fracture
r-Phase

1. Introduction microstructure and mechanical properties of martensitic and


duplex stainless steel welds [9–13], few is known about the weld
The 316LN austenitic stainless steel has been the backbone joints in austenitic stainless steel. Thus, their PWHT process must
structural material for many components due to its increase of be done carefully and observation of their following changes must
strength at cryogenic temperature and the nitrogen stabilizes the be closely studied to avoid the detrimental effects.
austenitic phase. However, the relatively high contents of chro- The present investigation was concerned with an evaluation of
mium and molybdenum, which improve the corrosion resistance the effect of post weld heat treatment at 600 °C, 760 °C, 870 °C and
of these steels, make the austenite unstable in the temperature 920 °C on the microstructure, tensile properties and impact tough-
range of 650 °C to 900 °C with respect to formation of ness of 316LN austenitic stainless steel weldments conducted
chromium-rich carbides and intermetallic phases [1–4]. In particu- through TIG welding technique with 316LMn filler metals since
lar, the presence of the r-phase, which is hard and brittle, harm- the wires are expected to provide a fully austenitic microstructure
fully affects the mechanical properties by creating local in the weld. The correlation between the changes in the
embrittlement and forming microcracks at the r/c-phase inter- microstructure during aging treatment, and impact toughness of
faces during loading. the investigated materials was assessed in order to obtain the opti-
The 316LN austenitic stainless steel used in ITER components is mum PWHT temperature for reducing the residual stress in the
often welded, such as the cases of superconducting magnets of the weld and assure the manufacturing precision.
TF(Toroidal coil) and CC(Correction coil) [5–8]. The residual stress
and deformation of these components caused by welding and
machining should be closely monitored during fabrication. Obvi- 2. Experimental
ously, the stress relieving after the welding is a critical process to
insure the manufacturing precision. Post weld heat treatment The 316LN austenitic stainless steel plates were manufactured
(PWHT) was considered as a feasible method of reducing the resid- by TISCO(China) and the plates are solution-treated at 1050 °C
ual stress and of minimizing the strength gradient across the weld for 140 min and water quenched. The chemical compositions of
joint. Many papers have reported the effect of PWHT on 316LN and its filler metal ER 316LMn (1.4455) were shown in
Table 1 which detected by atomic emission spectrometer, and
the mechanical properties of the base metal at room temperature
⇑ Corresponding author. is shown in Table 2. The XRD analysis of the base metal shows
E-mail address: fangchao@ipp.ac.cn (C. Fang). the single austenitic phase, no carbide or nitride was found in

http://dx.doi.org/10.1016/j.cryogenics.2017.02.001
0011-2275/Ó 2017 Elsevier Ltd. All rights reserved.
2 J. Xin et al. / Cryogenics 83 (2017) 1–7

Table 1
Chemical composition of base material (316LN) and filler material (ER 316LMn).

C Cr Ni Si Mn Mo N P S Co Nb B Fe
316LN 0.014 16.46 12.98 0.51 1.70 2.10 0.14 0.012 0.002 0.03 0.011 0.001 Balance
ER316LMn 0.009 20.3 15.5 0.49 7.0 2.9 0.17 0.01 0.005 – – – Balance

Table 2
Mechanical properties of the base metals.

Elongation [%] Yield strength [MPa] Ultimate tensile strength [MPa] Impact toughness [J/cm2]
316LN 55.0 352 665 >300

Fig. 1. XRD result of the 316LN austenitic stainless steel.

Fig. 1. The butt joints of 360  150  35 mm 316LN plates were


welded by TIG with the welding parameters which shown in the
Table 3 and the welding groove is shown in Fig. 2. The shield gas
was Argon and the maximum inter-pass temperature was strictly
controlled below 80 °C. The joints were held at temperatures of
600, 760, 870 and 920 °C in the RVSB-7816 vacuum furnace for
1 h, and then cooled at ambient temperature in the air. The
microstructure of joints and basic metal were analyzed with opti-
cal microscopy (OM), scanning electron microscopy (SEM, SU8020)
Fig. 2. Groove design of welding joint.
with energy dispersion system (EDS) techniques. The phases in the
different PWHT temperature of the 316LN weldments were ana-
lyzed by using a D8 ADVANCE X-ray diffractometer with Cu Ka ting process. The dimensions of the samples extracted from the
radiation of wavelength 1.544 Å. joints were shown in Fig. 3. The tensile test was performed on
The tensile strength and impact toughness with Charpy V notch the WA-1000A electro-hydraulic universal testing machine, the
of different aging temperatures were investigated according to the impact test specimens were immersing in the liquid nitrogen and
EN ISO4136:2012 and EN ISO9016:2012 standards, respectively. then tested on the impact testing machine in few seconds. The
Impact test and cross-weld tensile specimens were extracted from fractured morphologies of weldments were characterized by SEM
the steady state region of the joints using the wire-electrode cut- and EDS.

Table 3
Process parameters of TIG welding,

Passes Voltage [V] Current [A] Flow rate [L/min] Welding speed [mm/min] Filler wire dia. [mm]
Root pass 8–15 140 10–15 100–140 2.4
Fill passes 8–15 180–200 10–15 100–140 2.4
Cover pass 8–15 140–160 10–15 100–140 2.4
J. Xin et al. / Cryogenics 83 (2017) 1–7 3

Fig. 3. Test specimen dimensions: (a) tensile test specimen; and (b) Charpy V-notch impact test specimen.

3. Results and discussion They are mainly comprised of one phase (austenite) without clear
evidence of the precipitations of the secondary phases (such as
3.1. Metallographic examination r-phase and M23C6) and inclusions due to their relatively low
contents. Thus, in order to detecting the precipitations in the
Fig. 4 shows the microstructure of the base metal and fusion grain boundaries, the SEM images of welding sample aged at
zone in the transverse joints under as-welded and PWHT condi- 870 °C is presented in Fig. 6(a). The significant feature of the
tions. Fig. 4(a) shows the typical microstructure of the 316LN base microstructure is the presence of precipitated phase at the grain
metal which indicates the single austenite phase containing twins, boundaries. The precipitations in the fusion zone after aging at
the grain size is floating with the maximum at 100 lm and the 870 °C have maximum size of 8 ± 0.5 lm in length and
minimum at 40 lm. Fig. 4(b) shows the microstructure of as- 1 ± 0.5 lm in thickness. The average chemical composition of
welded metal. According to the Creq/Nieq ratios which are calcu- the precipitated phase was determined by energy dispersive
lated by using the Schaeffler formula, the weld metals solidified spectrometer attached to scanning electron microscope which is
in A mode with the single austenite phase. It is observed that the shown in Fig. 6(b). The phase is rich in Cr and Mo, which is dif-
morphology of the austenite changes into cells and dendrites after ferent from the composition adjacent to the phase, and according
welding, the columnar dendrites grow along transverse direction, to the literature [14], a typical sigma phase composition for the
and the dimension of cells is very fine. It is hardly found that there AISI 316L steel type is 44% Fe - 29% Cr - 8% Mo. The content of
are any solidification grain boundaries (SGBs) resulting from the principal elements of the phase determined by EDS is almost
intersection of packets of subgrains in fusion zone of as-welded same to this value, and the precipitated phase can be inferred
joint. In addition, it is also hardly found that there are any particles to be the r phase.
in interdendritic region(Fig. 4b).The interdendritic region was The fact that there is enough time for sigma phase formations to
known as solidification subgrain boundary(SSGB) separating adja- occur during the aging, but the precipitations could not be detected
cent subgrains. Fig. 4(c–f) show the microstructures of fusion zone in the results of the XRD analysis indicates that the amount of such
with various aging temperatures. Comparing with the fusion zone precipitations is below 5% even though their presence was
of as-welded joint, the microstructure is slight change aging at observed in SEM examinations. It has been reported that small pre-
600 °C, however, the size of cells and dendrites in the fusion zone cipitations that form at amounts below 5% cannot be identified via
is increasing when aging at 760 °C, as shown in Fig. 4(c) and (d), the XRD pattern [10].The mechanism of sigma phase nucleation is
respectively. As aging temperature increases, there are many SGBs still a matter of controversy and depends on the amount of delta
and quantities of black particles at SSGBs are appearing when ferrite. The delta ferrite content of the fusion zone plays an impor-
aging at 870 °C and 920 °C, as shown in Fig. 4(e) and (f). In addition, tant role in determining fabrication and service performance of the
the subgrains are less evident than that of the as-welded joint and welded structures [15]. For the 316LN austenitic stainless steel
aging at low temperatures shown in Fig. 4(b–d). While, the weld, the welding filler material was ER316LMn since the rods
migrated grain boundaries (MGBs) were found when aging at are expected to provide a fully austenitic microstructure in the
higher temperatures of 870 °C and 920 °C, the MGBs were charac- weld. The nucleation of the sigma phase is limit and the high con-
terized by a high impurity level and misorientation that leads to tent of nitrogen in the 316LN austenitic stainless steel will also
instability. And the secondary phase may be precipitated in these retard sigma formation. Further, the diffusion rates of the alloying
grain boundary. elements in the ferrite are about 100 times faster than in the
Fig. 5 shows the effect of the different aging temperatures on austenite [12]. Thus, the quantity of the sigma phase is exhibited
the XRD patterns in the fusion zones of the 316LN welding joints. at a very low level in the welds.
4 J. Xin et al. / Cryogenics 83 (2017) 1–7

(a) (b)

Cells
Dendrites

100μm 100μm

(c) (d)

100μm 100μm

(e) (f)

100μm 100μm

Fig. 4. Microstructure of fusion zone (a) base metal, (b) as-welded, (c) 600 °C, (d) 760 °C, (e) 870 °C and (f) 920 °C.

3.2. Tensile property of 316LN austenitic stainless steel welds

Fig. 7 shows the measured tensile properties at room temper-


ature (RT) of the as-welded and PWHT joints. For all samples
properties were above specified values at RT (Rp0.2 > 250 MPa,
Rm > 480 MPa, A > 35% with a target of 40%)[16]. As compared
to the base metal list in Table 2, the yield strength of test sam-
ples of as welded and different PWHT aging are determined to
be 380 MPa which is larger than the 352 MPa of base metal,
while their tensile strength are about 630 MPa, reaching the
95% of the basic metal. The yield and tensile values of the PWHT
samples are nearly the same, this indicates that the PWHT tem-
perature has less effect on the tensile properties. But the elonga-
tion of the samples exhibited improvement as the PWHT
temperatures increasing which is due to the reduction of the
residual stress in the samples. Also the fractures of all samples
are located at the base metal, this demonstrated that welding
parameters and heat treatment temperatures applied on the
Fig. 5. XRD result of the 316LN stainless steel weld joint and after PWHT. plates are appropriate.
J. Xin et al. / Cryogenics 83 (2017) 1–7 5

(a) (b)

Fig. 6. SEM micrographs of 316LN austenitic stainless steel weld aged at 870 °C.

Fig. 7. Tensile properties of the as-welded and PWHT samples at RT.

3.3. Impact property of 316LN austenitic stainless steel welds

The results of the Charpy V-notch impact test samples of fusion


zone in as-welded and different PWHT aging conditions are shown
in Fig. 8 (at 77 K). The tendency of impact toughness for weldments
of these tested samples at first showed an increase with increasing
temperature. However, this trend later reversed and toughness
decreased with increasging temperature. The impact toughness
of weldments after aging at 600 °C and 760 °C are larger when
compared to the as-welded condition, the toughness value are
108 J/cm2 and 123.6 J/cm2 which exceeded the value of as-
welded weldment of 103.8 J/cm2. As temperature continue to
increasing, the impact toughness is drastically decreased. The loss
of impact toughness for 870 °C and 920 °C weld is 24.1% and 39.1%,
respectively. For as-welded condition, the internal residual stresses
caused by the welding leading to a reduction in the impact tough-
ness of the weldment. As the aging temperature increasing, the
stress relieving effect is increasing, thus, the impact toughness
value of weldments aging at 600 °C and 760 °C are higher than
Fig. 8. The impact toughness of the 316LN austenitic stainless steel welds at 77 K.
as-welded condition. However, as the aging temperature continue
to increasing, the embrittlement sigma phase significantly deterio-
rated the impact toughness of the weldments, result in the Fig. 9 shows the SEM fractography of impact test samples per-
decreasing impact toughness as the aging temperature increasing formed at 77 K for original as-welded materials and PWHT welds.
to 870 °C and 920 °C. The fracture mode of all samples tested at 77 K displaying fibrous
6 J. Xin et al. / Cryogenics 83 (2017) 1–7

(a) (b)

2μm 2μm

(c) (d)

2μm 2μm

(e)

2μm

Fig. 9. SEM micrographs of the fractured impact test samples of TIG austenitic stainless steel welds (a) as-welded, (b) 600 °C, (c) 760 °C, (d) 870 °Cand (e) 920 °C.

fractures with typical dimples and without cleavage. Fig. 9(a) is the brittle phase is distributed in the austenite matrix. The chem-
representative of the fracture surfaces of as-welded weldment, ical composition of the precipitates determined by EDS corre-
the typical dimple appearance associated to ductile-dimple frac- sponding to the microstructure observation in Fig. 6. According
ture with a high microvoid density can be observed. This may be to the result of EDS spectrum, the brittle phase is also rich in Cr
attributed to the existence of an all austenite microstructure which and Mo, which infered to be r phase.
shows a good toughness. Meanwhile the PWHT weldments at
600 °C and 760 °C show the same fracture mode to the as- 4. Conclusion
welded weldment without any precipitate particles. As the PWHT
temperature increases, the dimples and microvoids became small In this investigation, the microstructure and mechanical prop-
and shallow, which indicates the deterioration of toughness. This erties of 316LN austenitic stainless steel weldments subjected to
could be reasoned out by the formation of precipitates which were different PWHT temperature were studied, the main conclusions
observed from the microstructure analysis. It is also evident from are summarized below:
the SEM fractographs, these precipitates are rather brittle and pre-
sent numerous secondary cracks on fracture surface. However, the (1) It is hardly found that there are any precipitates in the fusion
PWHT at 870 °Cand 920 °C weld samples show ductile fracture zone of as-welded and aging at 600 °Cand 760 °C, and the
mode in general. Although precipitates are observed on both sam- SGBs and MGBs and precipitated phase are found at the
ples as shown in fig. 9(d) and (e), dimples at the periphery of these higher aging temperatures of 870 °C and 920 °C, and is
precipitates are observed on the fracture surface which presents inferred to be the r phase since the chemical composition
ductile dimples in nature. is detected by EDS.
The SEM equipped with an energy dispersive spectrometer was (2) The fractures of the tensile sample are all located at the base
also applied for the observation of the precipitates and the analysis material. The PWHT aging enhanced the elongation and has
of its composition on the fracture surface. As can be seen in Fig.10, no detrimental effect on the tensile strength.
J. Xin et al. / Cryogenics 83 (2017) 1–7 7

(a) (b)

2μm

(c) (d)

2μm

Fig. 10. EDS spectrum of precipitates observed on fracture surfaces (a) (b) PWHT at 870 °C, (c) (d) PWHT at 920 °C.

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