Effects of Reversed Austenite on the Cryogenic Impact Toughness of 0Cr16Ni5Mo1 Super Martensitic Stainless Steel

doi:10.11900/0412.1961.2023.00100

Acta Metall Sin

2025, Vol. 61

Issue (5): 687-698 DOI: 10.11900/0412.1961.2023.00100

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Effects of Reversed Austenite on the Cryogenic Impact Toughness of 0Cr16Ni5Mo1 Super Martensitic Stainless Steel

SONG Yisi¹^,², LIAO Yu¹, LI Chuanwei¹^,²(

), CHEN Yihua¹, GU Jianfeng¹^,²(

)

1 Institute of Materials Modification and Modelling, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China
2 Shanghai Key Laboratory of Materials Laser Processing and Modification, School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China

Cite this article:

SONG Yisi, LIAO Yu, LI Chuanwei, CHEN Yihua, GU Jianfeng. Effects of Reversed Austenite on the Cryogenic Impact Toughness of 0Cr16Ni5Mo1 Super Martensitic Stainless Steel. Acta Metall Sin, 2025, 61(5): 687-698.

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Abstract

The reversed austenite obtained through a tempering process can effectively improve the toughness and ductility of super martensitic stainless steel (SMSS). Overcoming the trade-off between thermal stability and quantity of the reversed austenite is the key to improving the cryogenic impact toughness of SMSS. In this study, the mechanical properties at room temperature and cryogenic impact toughness at -196 ^oC of 0Cr16Ni5Mo1 SMSS after quenching and tempering (QT) were investigated, along with quenching, intercritical annealing, and tempering (QIT) processes. Reverse transformation behavior during the heat treatment was studied using a thermal dilatometer, and the microstructure evolution was characterized by XRD, EBSD, and TEM. Additionally, the effect of reversed austenite on cryogenic impact toughness was extensively analyzed. The results showed that full martensite was obtained in 0Cr16Ni5Mo1 SMSS after quenching at 1100 ^oC. The volume fraction of reversed austenite in the QT samples tempered at 620 ^oC was found to be 16.4%, which decreased to 5.0% after cryogenic treatment with liquid nitrogen, and the cryogenic impact toughness of the QT samples was obtained to be only 36.4 J/cm². The microstructure of samples after intercritical annealing at 680 ^oC mainly consisted of Ni-poor tempered martensite and Ni-rich fresh martensite. Furthermore, the volume fraction of reversed austenite in the QIT samples increased to 23.8% during the subsequent tempering process at 620 ^oC while the plasticity increased by 6% and the strength decreased by 7% at room temperature. The average Ni content of reversed austenite in the QIT samples reached 13% (mass fraction), which considerably improved the thermal stability of reversed austenite. Moreover, ~18.3% (volume fraction) reversed austenite remained stable in QIT samples at -196 ^oC, thereby substantially improving the cryogenic impact toughness to 115.4 J/cm² by absorbing the impact energy through transformation into martensite. The impact fracture of the QIT samples was dominated by dimples, but there remained a little quasicleavage morphology indicating a mixed fracture mode.

Key words: super martensitic stainless steel cryogenic impact toughness reversed austenite intercritical annealing

Received: 09 March 2023

ZTFLH:

TG142.1

Fund: National Natural Science Foundation of China(52171042);National Science and Technology Major Project of China(J2019-VI-0004-0117)

Corresponding Authors: LI Chuanwei, associate professor, Tel: (021)34201934, E-mail: li-chuanwei@sjtu.edu.cn;
GU Jianfeng, professor, Tel: (021)34203743, E-mail: gujf@sjtu.edu.cn

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	SONG Yisi
	LIAO Yu
	LI Chuanwei
	CHEN Yihua
	GU Jianfeng

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https://www.ams.org.cn/EN/10.11900/0412.1961.2023.00100 OR https://www.ams.org.cn/EN/Y2025/V61/I5/687

Fig.1 Schematics of quenching + tempering (QT) (a) and quenching + intercritical annealing + tempering (QIT) (b) heat treatment processes (A_c1 and A_c3 are start and end temperatures of austenite transformation, respectively)

Fig.2 Low (a-d) and high (e-h) magnified SEM images of 0Cr16Ni5Mo1 super martensitic stainless steel samples under different heat treatment conditions
(a, e) as-quenched (b, f) QT (RA—reversed austenite) (c, g) quenching + intercritical annealing (QI) (d, h) QIT

Fig.3 TEM analyses of the as-quenched and QT 0Cr16Ni5Mo1 super martensitic stainless steel samples
(a) bright-field (BF) image with corresponding selected area electron diffraction (SAED) pattern (inset) of the as-quenched sample
(b) BF image and SAED pattern (inset) of the QT sample
(c) dark-field (DF) image of the QT sample using g = (

1 ¯ 1 1 ¯

) _γ as the operating reflections showing film-like RA
(d) EDS line scanning results along the arrow in Fig.3c
(e) element distribution mappings of Fig.3b
(f) HRTEM image corresponding to the marked area in Fig.3b
(g) magnified HRTEM image and fast Fourier transform (FFT) result of M₂₃C₆ carbides
(h) magnified HRTEM image and FFT result of RA

Fig.4 TEM analyses of the QI and QIT samples
(a) BF image of QI sample, the Ni contents at the marked points were measured by EDS
(b) DF image and SAED pattern (inset) of QI sample showing tempered martensite (TM) and fresh martensite (FM)
(c) element distribution mappings of Fig.4a
(d) BF image of QIT sample
(e) DF image showing and SAED pattern (inset) of QIT sample using g = (

1 1 ¯ 1

) _γ as the operating reflections showing film-like RA
(f) DF image of QIT sample using g = (

110

) _α as the operating reflections showing TM
(g) element distribution mappings of Fig.4d
(h) EDS line scanning results along the arrow in Fig.4e

Fig.5 Room temperature XRD spectra of 0Cr16Ni5Mo1 super martensitic stainless steel samples under different heat treatment conditions (V_γ —volume fraction of RA)

Fig.6 Engineering stress-strain curves of 0Cr16Ni5Mo1 super martensitic stainless steel samples under different heat treatment conditions

Fig.7 Load and absorbed energy versus deflection curves of as-quenched (a), QT (b), QI (c), and QIT (d) 0Cr16Ni5Mo1 super martensitic stainless steel samples at 25 and -196 ^oC

Fig.8 Impact energies at 25 and -196 ^oC of 0Cr16Ni5-Mo1 super martensitic stainless steel samples under different heat treatment conditions

Table 1 Mechanical properties of 0Cr16Ni5Mo1 super martensitic stainless steel samples under different heat treatment conditions

Fig.9 Low (a, c, e, g) and high (b, d, f, h) magnified SEM images of impact fracture of QT (a, b, e, f) and QIT (c, d, g, h) samples at 25 ^oC (a-d) and -196 ^oC (e-h)

Fig.10 Dilatometer curves of QT (a) and QIT (b) samples (M_s—start temperature of martensite transformation)

Fig.11 Gibbs free energy (ΔG) as a function of Ni content at 620 ^oC (a) and 680 ^oC (b) for bcc and fcc phases in 0Cr16Ni5Mo1 super martensitic stainless steel samples

Fig.12 XRD spectra of QT and QIT samples after subject to liquid nitrogen

Fig.13 SEM images showing longitudinal section of impact fracture of QT (a) and QIT (b) samples at -196 ^oC; EBSD phase maps taken at the impact fracture sites as marked in Fig.13a (c) and Fig.13b (d); EBSD phase map taken at the area ~200 μm from the fracture surface (e); and EBSD phase map taken at the undeformed end of the specimen (f)

1	Lei X W, Feng Y R, Zhang J X, et al. Impact of reversed austenite on the pitting corrosion behavior of super 13Cr martensitic stainless steel [J]. Electrochim. Acta, 2016, 191: 640
2	Anselmo N, May J E, Mariano N A, et al. Corrosion behavior of supermartensitic stainless steel in aerated and CO₂-saturated synthetic seawater [J]. Mater. Sci. Eng., 2006, A428: 73
3	Mesquita T J, Chauveau E, Mantel M, et al. Corrosion and metallurgical investigation of two supermartensitic stainless steels for oil and gas environments [J]. Corros. Sci., 2014, 81: 152
4	Bilmes P D, Solari M, Llorente C L. Characteristics and effects of austenite resulting from tempering of 13Cr-NiMo martensitic steel weld metals [J]. Mater. Charact., 2001, 46: 285
5	Zou D N, Han Y, Yan D N, et al. Hot workability of 00Cr13Ni5Mo2 supermartensitic stainless steel [J]. Mater. Des., 2011, 32: 4443
6	Della Rovere C A, Ribeiro C R, Silva R, et al. Microstructural and mechanical characterization of radial friction welded supermartensitic stainless steel joints [J]. Mater. Sci. Eng., 2013, A586: 86
7	Woollin P, Kostrivas A. Use of supermartensitic stainless steel pipe for offshore flowline applications [A]. 25th International Conference on Offshore Mechanics and Arctic Engineering [C]. Hamburg: ASME, 2006: 565
8	Liu Z B, Liang J X, Su J, et al. Research and application progress in ultra-high strength stainless steel [J]. Acta Metall. Sin., 2020, 56: 549
	刘振宝, 梁剑雄, 苏杰等. 高强度不锈钢的研究及发展现状 [J]. 金属学报, 2020, 56: 549 doi: 10.11900/0412.1961.2019.00453
9	Ye D, Li J, Jiang W, et al. Effect of Cu addition on microstructure and mechanical properties of 15%Cr super martensitic stainless steel [J]. Mater. Des., 2012, 41: 16
10	Song Y Y, Ping D H, Yin F X, et al. Microstructural evolution and low temperature impact toughness of a Fe-13%Cr-4%Ni-Mo martensitic stainless steel [J]. Mater. Sci. Eng., 2010, A527: 614
11	Song Y Y, Li X Y, Rong L J, et al. The influence of tempering temperature on the reversed austenite formation and tensile properties in Fe-13%Cr-4%Ni-Mo low carbon martensite stainless steels [J]. Mater. Sci. Eng., 2011, A528: 4075
12	Ma X P, Wang L J, Liu C M, et al. Microstructure and properties of 13Cr5Ni1Mo0.025Nb0.09V0.06N super martensitic stainless steel [J]. Mater. Sci. Eng., 2012, A539: 271
13	Tabatabae B A, Ashrafizadeh F, Hassanli A M. Influence of retained austenite on the mechanical properties of low carbon martensitic stainless steel castings [J]. ISIJ Int., 2011, 51: 471
14	Yang D. Effect of tempering process on low temperature impact toughness of 13Cr4NiMo Low carbon martensitic stainless steel [D]. Nanning: Guangxi University, 2020
	杨东. 回火工艺对13Cr4NiMo低碳马氏体不锈钢低温冲击韧性的影响 [D]. 南宁: 广西大学, 2020
15	Song Y Y. Formation mechanism of the reversed austenite in 0Cr13Ni4Mo stainless steel [D]. Shenyang: Institute of Metal Research, Chinese Academy of Sciences, 2011
	宋元元. 0Cr13Ni4Mo不锈钢中逆变奥氏体的相变机制 [D]. 沈阳: 中国科学院金属研究所, 2011
16	Wen Z M. Study on composition, microstructure and properties of high strength martensitic stainless steel used in low-temperature environment [D]. Kunming: Kunming University of Science and Technology, 2011
	文志旻. 低温用高强度马氏体不锈钢成分、组织及性能的研究 [D]. 昆明: 昆明理工大学, 2011
17	Qiu X Y F, Yang Z Y, Ding Y L. Solid solution treatment for improving cryogenic temperature toughness of Cr-Ni-Mo-Ti maraging stainless steel [J]. Heat Treat. Met., 2022, 47(1): 44
	邱旭扬帆, 杨卓越, 丁雅莉. 提高Cr-Ni-Mo-Ti马氏体时效不锈钢超低温韧性的固溶处理工艺 [J]. 金属热处理, 2022, 47(1): 44 doi: 10.13251/j.issn.0254-6051.2022.01.008
18	Ji Y R, Yang Z Y, Tan H L, et al. Heat treatment process for improving cryogenic toughness of Cr-Ni-Co-Mo maraging stainless steel [J]. Heat Treat. Met., 2021, 46(10): 133 doi: 10.13251/j.issn.0254-6051.2021.10.023
	吉昱睿, 杨卓越, 谭红琳等. 提高Cr-Ni-Co-Mo马氏体时效不锈钢超低温韧性的热处理工艺 [J]. 金属热处理, 2021, 46(10): 133 doi: 10.13251/j.issn.0254-6051.2021.10.023
19	Luo H W, Shi J, Wang C, et al. Experimental and numerical analysis on formation of stable austenite during the intercritical annealing of 5Mn steel [J]. Acta Mater., 2011, 59: 4002
20	Shi J, Sun X J, Wang M Q, et al. Enhanced work-hardening behavior and mechanical properties in ultrafine-grained steels with large-fractioned metastable austenite [J]. Scr. Mater., 2010, 63: 815
21	Han G, Shang C J, Xie Z J, et al. On the thermal and mechanical stability of reverted austenite by intercritical tempering [J]. Mater. Lett., 2021, 291: 129457
22	Wang C J, Liang J X, Liu Z B, et al. Effect of metastable austenite on mechanical property and mechanism in cryogenic steel applied in oceaneering [J]. Acta Metall. Sin., 2016, 52: 385
	王长军, 梁剑雄, 刘振宝等. 亚稳奥氏体对低温海工用钢力学性能的影响与机理 [J]. 金属学报, 2016, 52: 385 doi: 10.11900/0412.1961.2015.00312
23	Hou W, Liu Q D, Gu J F. Nano-sized austenite and Cu precipitates formed by using intercritical tempering plus tempering and their effect on the mechanical property in a low carbon Cu bearing 7Ni steel [J]. Mater. Sci. Eng., 2020, A780: 139186
24	Song Y Y, Li X Y, Rong L J, et al. Formation of the reversed austenite during intercritical tempering in a Fe-13%Cr-4%Ni-Mo martensitic stainless steel [J]. Mater. Lett., 2010, 64: 1411
25	Hu J, Du L X, Wang J J, et al. Structure-mechanical property relationship in low carbon microalloyed steel plate processed using controlled rolling and two-stage continuous cooling [J]. Mater. Sci. Eng., 2013, A585: 197
26	Zhang S H, Wang P, Li D Z, et al. Investigation of the evolution of retained austenite in Fe-13%Cr-4%Ni martensitic stainless steel during intercritical tempering [J]. Mater. Des., 2015, 84: 385
27	Xiong X C, Chen B, Huang M X, et al. The effect of morphology on the stability of retained austenite in a quenched and partitioned steel [J]. Scr. Mater., 2013, 68: 321
28	Matsuoka Y, Iwasaki T, Nakada N, et al. Effect of grain size on thermal and mechanical stability of austenite in metastable austenitic stainless steel [J]. ISIJ Int., 2013, 53: 1224
29	Kang J, Wang C, Wang G D. Microstructural characteristics and impact fracture behavior of a high-strength low-alloy steel treated by intercritical heat treatment [J]. Mater. Sci. Eng., 2012, A553: 96

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