4achieving Continuous Cold Rolling of Martensitic Stainless Steel Via Online Induction Heat Treatment

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Materials Science & Engineering A 739 (2019) 415–426

Contents lists available at ScienceDirect

Materials Science & Engineering A


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

Achieving continuous cold rolling of martensitic stainless steel via online T


induction heat treatment
Kangda Haoa, Ming Gaob, , Chen Zhangc, Run Wua, Xiaoyan Zengb

a
The State Key Laboratory of Refractories and Metallurgy, Wuhan University of Science and Technology, Wuhan 430081, China
b
Wuhan National Laboratory for Optoelectronics (WNLO), Huazhong University of Science and Technology, Wuhan 430074, China
c
The Institute of Technological Sciences, Wuhan University, Wuhan 430072, China

ARTICLE INFO ABSTRACT

Keywords: The continuous cold rolling of martensitic stainless steel (MSS) has not been achieved so far because of the poor
Hybrid welding weld toughness caused by the occurrence of the brittle martensite. How to improve the toughness of MSS weld is
Heat treatment then one of the most concerned challenges in steel rolling industries. In this paper, the toughness of the MSS weld
Stainless steel was increased to meet the rolling requirement by introducing the online induction heat treatment into laser-arc
Continuous rolling
hybrid welding. The heat treatment parameters were optimized, which was the heating temperature of 650 °C
Martensite
Toughness
and the holding time longer than 5 s. The weld toughness characterized by Erichsen cupping value was increased
from 5.7 mm to 8.7 mm, while the bearable rolling reduction was increased from 25% to 75%. The micro-
structure-toughness-bearable rolling reduction relationship was established according the experimental results.
The mechanism of the microstructure transformation was explained by the thermodynamic calculation of aus-
tenite stability, which is dominated by the diffusion behavior of alloying elements. The toughness improvement
was discussed according to the microstructure transformation and the crack propagation behaviors, which is
closely related to the austenite content and the martensite with high-angle misorientation.

1. Introduction The post weld heat treatment (PWHT) is effective to improve the
toughness of MSS weld [11]. During PWHT, the reversed austenite with
Continuous cold rolling of martensitic stainless steel (MSS) has great excellent thermo-stability forms among the martensite laths, which is
profit margins because of good mechanical properties, moderate cor- beneficial to improve the weld toughness by relieving the concentrated
rosion resistance and low cost, which is significant for the steel in- stress [12]. For the weld of 13Cr4NiMo MSS with PWHT, the elongation
dustries. Generally, the brittleness of the heat-affected zone (HAZ) ap- increased from 10.8% to 18.3% with the content of austenite increased
pears in arc welds because of big heat input, while that of the fusion from 7.6% to 16.1% [13]. In the friction welding of AISI 431 MSS, the
zone (FZ) easily occurs in laser welds because of the lack of me- elongation of heat-treated sample increased by 41.7% in comparison of
tallurgical control of alloying elements [1–3]. Thus, the weld breakage as-welded sample, while the impact energy increased from 4 J to 68 J.
is easily occurred during the continuous cold rolling of the MSS because Correspondingly, the fracture mode changed from the cleavage fracture
of its poor weld toughness. to the quasi-cleavage fracture including some dimples [14]. Moreover,
Fortunately, laser-arc hybrid welding could obtain better quality there were also many researches employing two-step tempering on the
[4–6] by integrating the small heat input of laser welding and the MSS weld to obtain more reversed austenite [15,16].
strong metallurgical control of arc welding [7,8]. On this basis, our However, no relevant research has paid attention to laser-arc hybrid
previous studies demonstrated that the HAZ toughness could be in- welding, especially aiming to achieve continuous rolling of the MSS.
creased by decreasing heat input, and the FZ toughness could be im- The researches above are carried out by traditional equipment for heat
proved employing Ni-rich filling wire [9,10]. It causes the rolling of treatment, which is large and time-consuming, and is hard to be in-
MSS weld possible, but the bearable reduction is limited, which results tegrated into the automatic rolling line. Relatively, induction heat
in frequent breakage during rolling under severe condition yet. treatment can overcome the above problems with smaller heater and
Therefore, how to further improve the weld toughness and the rolling faster heating speed. Thus, a series of experiments were carried out to
stability became the new challenge. further improve the bearable rolling reduction of AISI 420 MSS weld in


Corresponding author.
E-mail address: mgao@mail.hust.edu.cn (M. Gao).

https://doi.org/10.1016/j.msea.2018.10.071
Received 22 August 2018; Received in revised form 13 October 2018; Accepted 15 October 2018
Available online 16 October 2018
0921-5093/ © 2018 Elsevier B.V. All rights reserved.
K. Hao et al. Materials Science & Engineering A 739 (2019) 415–426

was carried out after welding. The heating temperature (T) was mea-
sured by infrared thermometer, while the holding time (t) was calcu-
lated by Eq. (1). The heat treatment parameters are shown in Table 1.
t = L / vi (1)

where, L is the length of the induction coil, vi is the moving speed of the
coil.
The Erichsen cupping test and tensile test were repeated for three
times according to the standard of ISO 20482-2003 and ASTM E8/
(E8M)-11, respectively. The rolling experiment with 75% reduction was
carried out using a two-high rolling mill. The crack morphologies of
Erichsen and rolling samples were observed by FEI Quanta-200 en-
vironmental scanning electron microscope (SEM).
In order to obtain a good display effect of microstructure, the FZ of
weld upper and lower part was electrolytically and chemically etched,
Fig. 1. Diagrammatic drawing of experimental set-up. respectively. The HAZ was two-step etched. The EBSD samples were
electrolytically polished. The detailed procedures are introduced in
reference [10]. The microstructure was observed by environmental
Table 1
Online induction heat treatment parameters, where T is heating temperature, t
SEM, and the EBSD samples were tested by an EDAX-TSL OIM system
is holding time, vi is moving speed of the induction coil. with step size of 0.15 µm.

Weld no. #0 #1 #2 #3 #4 #5 #6 #7 #8 #9
3. Results
T (°C) / 350 550 650 750 850 650 650 650 650
t (s) / 2.5 2.5 2.5 2.5 2.5 5 10 15 20 3.1. Weld toughness
vi (m/min) / 3.6 3.6 3.6 3.6 3.6 1.8 0.9 0.6 0.45

3.1.1. Erichsen cupping toughness


As shown in Fig. 2, almost all the samples crack along the BM during
this paper. Relevant mechanisms were discussed in detail. The results
the Erichsen cupping test, except for the weld with the T of 850 °C and
would be significant for the optimization design of continuous rolling of
the t of 2.5 s. Under given t of 2.5 s, the Erichsen value increases to
the MSS, especially the designs of the heat treatment parameters and
maximum of 6.9 mm at 650 °C, about 19.1% higher than that of the as-
the subsequent rolling parameter.
welded sample, and then decreases to 3.6 mm when the T reaches
850 °C. Under given T of 650 °C, the Erichsen value continuously in-
2. Material and methods creases to 8.7 mm when the t prolongs from 2.5 s to 20 s, 45.9% higher
than that of the as-welded sample.
The base metal (BM) was AISI 420 MSS (Fe-13.29Cr-0.19C, wt%)
sheet with 500 mm (length) × 100 mm (width) × 4 mm (thickness) in 3.1.2. Cold rolling toughness
size. The filling wire of ER NiCr-3 (65.8 Ni-21.3Cr- 8.8Mo-4.9 Nb, wt%) Generally, laser-arc hybrid weld is featured by a wine-cup shape
was selected. After milling and cleaning, the sheets were butt-welded consisting of wide upper arc zone (ArcZ) and narrow lower laser zone
with zero-gap. (LaserZ) [17]. As shown in Fig. 3, the as-welded sample only suffers
A Fanuc robot, an IPG fiber laser and a Fronius arc welder were reduction of 25%, then cracks along the fusion line with reduction of
employed for laser-arc hybrid welding. On this basis, a Bamac induction 35%. However, the heat treated sample can suffer a larger reduction of
power was employed for online PWHT, as shown in Fig. 1. The PWHT 75% because of the improvement of the toughness

Fig. 2. Erichsen cupping test results and crack locations, (a) effect of heating temperature with the holding time of 2.5 s, (b) effect of holding time at the heating
temperature of 650 °C.

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Fig. 3. Crack morphologies of the as-welded sample, (a) overview of sample with 25% reduction, (b) overview of sample with 35% reduction, (c) enlarged view of
area A, where Crack-FL is crack at fusion line.

As shown in Figs. 4 and 6a, under the given t of 2.5 s, the cracking but nearly irrelevant to the t, and can be divided into two stages with
tendency reaches the minimum when the T is 650 °C. The crack length threshold T of 650 °C. It keeps at about 60% when the T keeps below
reduces from 0.259 mm to 0.051 mm. When the T reaches 850 °C, the 650 °C, and linearly decreases to 49.2% when the T increases to 850 °C.
crack length reversely increases to 0.95 mm. On the other hand, under Generally, the grain boundaries with high-angle misorientation de-
the given T of 650 °C, the cracking tendency is thoroughly suppressed crease the ductile-brittle transition temperature, hinder the crack pro-
when the t is longer than 5 s, as shown in Figs. 5 and 6b. pagation, and then improve the toughness [19–21].
Thus, the optimized PWHT parameters free of rolling crack are
confirmed as the T of 650 °C and the t longer than 5 s. In this case, the 3.2.3. HAZ microstructure after heat treatment
Erichsen value reaches more than 7.2 mm. It is noted that the As shown in Fig. 12, the HAZ microstructures of all the samples are
prolonging of the t longer than 5 s increases the Erichsen value, but has similar, which are differed with different tempering degree of the
no effect on the visible cracking behavior under the reduction of 75%. martensite. Under the given t of 2.5 s, the grain boundaries of the
martensite become fuzzy when the T increases below 650 °C, indicating
3.2. Microstructure characteristics an enhanced tempering effect. However, the boundaries become dis-
tinguishable when the T increases to 850 °C, indicating a weakened
3.2.1. Microstructure of as-welded sample tempering effect. On the other hand, under the given T of 650 °C, the
As shown in Fig. 7, the ArcZ of the as-welded sample is almost to- martensite always keeps in the strong tempering state when the t pro-
tally composed of austenite, the HAZ is mainly composed of martensite, longs from 2.5 s to 20 s.
while the LaserZ is composed of martensite, some δ-ferrite, and bright As shown in Fig. 13, the CHM within the HAZ also can be divided
structures. The bright structures within the LaserZ are hard to be dis- into two stages with threshold of 650 °C, which is much similar with
tinguished between the carbide and the austenite in morphology be- that within the LaserZ. It keeps at about 60% when the T is below
cause the austenite always forms around the carbide [18]. It is noted 650 °C irrelevant to the t, and then linearly decreases to 47.2% when
that the austenite content of the ArcZ is much higher than that of the the T increases to 850 °C.
LaserZ because the austenite stabilized elements from the filling wire
prefer to stay at the ArcZ. 4. Discussion

3.2.2. Microstructure of heat-treated sample 4.1. Austenite formation


Above results confirm that the LaserZ and the HAZ are the weak
areas because of the formation of brittle martensite. Thus, the micro- The results mentioned above show that the rolling toughness is
structure and crystallographic characteristics of these areas are mainly mainly attributed to the formation of the austenite in the LaserZ formed
examined. during PWHT [22], which is beneficial to decrease the cracking ten-
As shown in Fig. 8, the LaserZ of the heat-treated samples are dency. During heating, the Cr element is depleted adjacent to the
composed of martensites, some granular and short-bar-shaped carbides martensite boundaries because of the formation of Cr-rich carbide [23].
or austenite. Among them, the austenite content reaches the maximum In this case, the reversed austenite forms from the martensite because of
of 23.4% at 650 °C under the given t of 2.5 s, and decreases to 4.1% the diffusion of element Ni to these areas [24,25]. Thus, the reversed
when the T increases to 850 °C, as shown in Figs. 9 and 10. Under the austenite is generally formed by diffusion [26], and its stability can be
given T of 650 °C, the austenite content continuously increases to 29.3% expressed by Eq. (2) [24].
with the rate slowing down when the t prolongs from 2.5 s to 20 s. G= G + E str + (2)
Except for the austenite content in the LaserZ, the content of mar-
tensite with high-angle misorientation (CHM) affects the rolling tough- where, ΔG is the critical driving force for the martensitic transforma-
ness as well. As shown in Fig. 11, the CHM is only dependent on the T, tion, ΔGγ→α is the corresponding Gibbs free energy, Estr is the elastic

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Fig. 4. Effects of heating temperature on the crack morphologies of the sample rolled with 75% reduction, (a) T = 350 °C, t = 2.5 s, (b) enlarged view of area B, (c)
enlarged view of area C, (d) T = 550 °C, t = 2.5 s, (e) enlarged view of area D, (f) T = 650 °C, t = 2.5 s, (g) enlarged view of area E, (h) T = 750 °C, t = 2.5 s, (i)
enlarged view of area F, (j) T = 850 °C, t = 2.5 s, (k) enlarged view of area G, where Crack-LZ is crack within LaserZ, Crack-FL is crack at fusion line.

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Fig. 5. Effects of holding time on crack morphologies of the sample rolled with 75% reduction, (a) T = 650 °C, t = 5 s, (b) T = 650 °C, t = 10 s, (c) T = 650 °C,
t = 15 s, (d) T = 650 °C, t = 20 s.

Fig. 6. Crack length of the sample rolled with 75% reduction, (a) effect of heating temperature with the holding time of 2.5 s, (b) effect of holding time at the heating
temperature of 650 °C.

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Fig. 7. As-welded microstructure, (a) ArcZ, (b) LaserZ, (c) HAZ, where M is martensite, A is austenite, F is ferrite, δ-F is δ ferrite, C is carbide, Inter-C is inter-granular
carbide, Intra-C is intra-granular carbide.

Fig. 8. SEM graph of the LaserZ microstructure, (a) T = 350 °C, t = 2.5 s, (b) T = 650 °C, t = 2.5 s, (c) T = 850 °C, t = 2.5 s, (d) T = 650 °C, t = 20 s.

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Fig. 9. Inverse pole figure (IPF) and phase map of the LaserZ microstructure, (a) T = 350 °C, t = 2.5 s, (b) T = 650 °C, t = 2.5 s, (c) T = 850 °C, t = 2.5 s, (d)
T = 650 °C, t = 20 s.

Fig. 10. Austenite content within the heat-treated samples, (a) effect of heating temperature with the holding time of 2.5 s, (b) effect of holding time at the heating
temperature of 650 °C.

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Fig. 11. Misorientation of the LaserZ, (a) misorientation distribution under varied heating temperature, (b) relationship between high-angle misoritation content and
heating temperature, (c) misorientation distribution under varied holding time, (d) relationship between high-angle misoritation content and holding time.

strain energy, γ is interface energy. It indicates that decreasing the According to Fig. 14a, the DNi-M can be divided into two stages with
ΔGγ→α, increasing the Estr or the γ can increase the ΔG, which is ben- critical temperature of 650 °C. It slightly increases from magnitude of
eficial to improve the stability of the austenite. 10–20 to 10–14 when the T increases from 350 °C to 650 °C, and then
The reversed austenite can be remained to room temperature at Ni- sharply increases to 10–11 when the T continuously increases to 850 °C.
rich areas since the enrichment of Ni can decrease the ΔGγ→α and in- The variation of the DNi-M with the T is well corresponding to the
crease the γ [24], which increases the stability. Thus, the formation of content of reversed austenite (CRVA). Thus, the formation of the re-
the reversed austenite is closely related to the diffusion behavior of versed austenite during heating can be illustrated.
element Ni [27,28], whose diffusion coefficient can be calculated by For the as-welded sample, the element Ni is mainly distributed in
Arrhenius equation, as expressed by Eq. (3) [29]. the retained austenite, as shown in Fig. 15a. When employing heat
treatment below 650 °C, the element Ni in the retained austenite
D = D0 exp( Q/RT ) (3)
slightly diffuses to and enriches in part of the martensite, which pro-
where, D is the element diffusion coefficient (cm2 s−1), D0 is the dif- motes the formation of reversed austenite during holding period, as
fusion constant (cm2 s−1), R is the ideal gas constant (J mol−1 K−1), T shown in Fig. 15b. At this stage, the content of reversed austenite
is the absolute temperature (K), Q is the activation energy of diffusion (CRVA) increases due to the diffusion of Ni with the T increasing. The
(J/mol). reversed austenite decreases the average concentration of the element
According to Eq. (3), the diffusion coefficient of element Ni in Ni, which promotes partly unstable martensite transforming to auste-
martensite (DNi-M) and austenite (DNi-A) can be calculated by Eq. (4) nite in the subsequent cooling period [31]. However, the transforming
and Eq. (5), respectively [30]. As shown in Fig. 14, the DNi-A is about rate is lower than the forming rate in general. Thus, the CRVA remained
three magnitudes smaller than the DNi-M at given temperature, which at room temperature increases with the T increasing below 650 °C yet.
can be ignored. Thus, the formation of reversed austenite is only de- On the other hand, when employing heat treatment above 650 °C, the
pendent on the DNi-M. reversed austenite forms substantially during holding period because of
DNi = 4.8 exp( 240000/ RT ) (4) the sharply increase of the DNi-M, as shown in Fig. 15c. The austenite
M
stability decreases significantly because of the reduction of the average
DNi A = 3.5 exp( 286000/ RT ) (5) Ni concentration. At this stage, almost all of the reversed austenite and

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Fig. 12. HAZ microstructure of the heat-treated samples, (a) T = 350 °C, t = 2.5 s, (b) T = 650 °C, t = 2.5 s, (c) T = 850 °C, t = 2.5 s, (d) T = 650 °C, t = 20 s, where
M is martensite, Inter-C is inter-granular carbide, Intra-C is intra-granular carbide, FZ is fusion zone, FGHAZ is fine-grained HAZ, T is heating temperature, t is
holding time.

partly retained austenite transform to martensite in the subsequent 650 °C. At this stage, the CRVA increases with the increase of the T,
cooling period, which results in the decrease of CRVA. which results in an enhanced effect to soften the martensite and de-
crease the stress concentration around the grain boundaries. The rolling
crack is then shortened and suppressed at 650 °C for 5 s with CRVA of
4.2. Toughness improvement 24.8%.
As shown in Fig. 16b, the rolling toughness is related to both the
During plastic deformation, the austenite is beneficial to soften the CRVA and the CHM when the T increases above 650 °C. At this stage, the
martensite with low dislocation density, decrease the stress con- decrease of the CRVA weakens the soften effect of the martensite, and
centration around the grain boundaries, and then increase the propa- the decrease of the CHM promotes the crack initiation and propagation.
gation resistance of the cleavage crack [32]. On the other hand, the Thus, the rolling toughness is decreased with the formation of the pe-
grain boundaries with high-angle misorientation play an important role netrating crack.
in increasing the crack propagation energy and suppressing the crack
propagation [20]. The experiments above show that the cracking be- 5. Conclusions
havior is mainly related to the T, but nearly irrelevant to the t. On the
basis of the above views and results, the toughness improvement me- (1) The weld toughness of the martensitic stainless steel (MSS) can be
chanism and cracking behavior could be explained as following. improved, and the continuous rolling of the MSS is achieved by
As shown in Fig. 16a, the rolling toughness is only related to the introducing induction heat treatment into laser-arc hybrid welding.
CRVA because the CHM keeps unchanged when the T increases below

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Fig. 13. Misorientation of the HAZ, (a) misorientation distribution under varied heating temperature, (b) relationship between high-angle misoritation content and
heating temperature, (c) misorientation distribution under varied holding time, (d) relationship between high-angle misoritation content and holding time.

Fig. 14. Relationship between diffusion coefficient and temperature, (a) DNi-M, (b) DNi-A.

The optimal heat treatment parameters are confirmed as heating (3) The formation of reversed austenite is closely related to the diffu-
temperature (T) of 650 °C and holding time (t) longer than 5 s. sion of Element Ni. The Element Ni slightly diffuses to and enriches
Comparing with the as-welded sample, the Erichsen value increases in part of martensite with the increase of the T below 650 °C, which
by larger than 26%, while the bearable reduction increases by two promotes the formation of reversed austenite and increases tough-
times. ness. When the T is above 650 °C, the reversed austenite sub-
(2) The content of high-misorientation martensite (CHM) within the stantially forms during heating due to sharply increased diffusion
weld keeps at about 60% except for the samples with the T above coefficient of Ni, which decreases the average Ni concentration,
650 °C. The content of reversed austenite (CRVA) increases to max- promotes the austenite with reduced stability transforming to
imum of 23.4% when the T increases to 650 °C under given t of martensite during cooling, and decreases the toughness.
2.5 s, and then continuously increases to 29.3% with the rate (4) The weld toughness is only related to CRVA when the T was lower
slowing down when the t prolongs to 20 s under 650 °C. than 650 °C because the CHM keeps constant. On the other hand, the

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Fig. 15. Schematic diagram of formation mechanism of reversed austenite under different heating temperature, (a) the as-welded sample, (b) the sample heat-treated
below 650 °C, (c) the sample heat-treated above 650 °C.

Fig. 16. Schematic diagrams of cracking behavior during rolling, (a) heating temperature below 650 °C, (b) heating temperature above 650 °C.

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