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Acta Metall Sin  2022, Vol. 58 Issue (9): 1199-1207    DOI: 10.11900/0412.1961.2021.00432
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Mechanical Properties and Creep Behavior of MX-Type Precipitates Strengthened Heat Resistant Martensite Steel
LI Xiaolin1(), LIU Linxi1, LI Yating1, YANG Jiawei1, DENG Xiangtao2, WANG Haifeng1
1.State Key Laboratory of Solidification Processing & Center of Advanced Lubrication and Seal Materials, Northwestern Polytechnical University, Xi'an 710072, China
2.State Key Laboratory of Rolling and Automation, Northeastern University, Shenyang 110819, China
Cite this article: 

LI Xiaolin, LIU Linxi, LI Yating, YANG Jiawei, DENG Xiangtao, WANG Haifeng. Mechanical Properties and Creep Behavior of MX-Type Precipitates Strengthened Heat Resistant Martensite Steel. Acta Metall Sin, 2022, 58(9): 1199-1207.

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Abstract  

There has been a push in the past few decades to increase the operating temperature of steam generators to the ultra-supercritical (USC) regime. This requires that creep-resistant alloys can operate at 650-700°C for 30 years. P91 and P92 steels are commercially applied in USC steam generator applications. However, these steels fail due to the coarsening of M23C6 and Laves phases during long-term service. Therefore, it is significant to restrict the formation of easily coarsened precipitates. In this study, a martensitic heat-resistant steel strengthened by single MX precipitates is designed using the Thermo-Calc software, as Fe-0.03C-10Cr-0.2Zr-0.3V. The yield strength, tensile strength, and elongation at room temperature are 266 MPa, 413 MPa, and 38%, respectively. The high-temperature hardnesses of specimens aged at 700oC for 1, 10, 100, and 1000 h were tested at 700oC after normalizing treatment, which illustrates that the high-temperature hardness of the specimens remains stable with increased aging time. In addition, TEM was used to characterize the precipitates in the heat-resistant steel aged for different times. It is found that with the increase of aging time (1-1000 h), the average size of the precipitates increases from 10.8 to 17.8 nm. The composition of MX precipitates in the specimens aged for 1000 h is Zr0.46Nb0.14C0.4 and the volume fraction is 0.29%. According to the creep test results, the threshold stresses at 650 and 700oC are 54.5 and 28.4 MPa, respectively.

Key words:  martensite heat-resistant steel      MX-type precipitate      creep behavior      threshold stress      CALPHAD technique     
Received:  15 October 2021     
ZTFLH:  TG113  
Fund: National Natural Science Foundation of China(52004224);China Postdoctoral Science Foundation(2020M683559)
About author:  LI Xiaolin, associated professor, Tel: (029)88460311, E-mail: xiaolinli@nwpu.edu.cn

URL: 

https://www.ams.org.cn/EN/10.11900/0412.1961.2021.00432     OR     https://www.ams.org.cn/EN/Y2022/V58/I9/1199

Fig.1  Phase diagrams of P91 steel (0.1C-9Cr-1Mo-0.22V-0.08Nb-0.3Ni-0.05N-0.23Si-0.04Mn) (a) and T alloy (0.1C-9Cr-0.22V-0.08Nb-0.05Zr-0.12Ti-1.2W-0.12Ni-0.8Mn-0.15Si) (b)
Fig.2  Schematics for composition design and screening process (V—volume fraction of phase)
Fig.3  Phase diagram (a) and step diagram (b) of the designed heat-resistant steel
Fig.4  OM (a) and TEM (b) images of Fe-0.03C-10Cr-0.2Zr-0.3V steel by HR + N treatment and aged at 700oC for 1 h (HR + N—hot rolling + normalizing at 1000oC for 1 h)
Fig.5  Morphologies and size distributions of precipitates (Stdev—standard deviation)
(a-f) TEM images (a-c) and size distributions (d-f) of precipitates formed in Fe-0.03C-10Cr-0.2Zr-0.3V steel aged at 700oC for 10 h (a, c), 100 h (b, e), and 1000 h (c, f) after HR + N treatment
(g-i) SEM (g, h) and TEM (i) images of Fe-0.03C-10Cr-0.2Zr-0.3V steel aged at 700oC for 1000 h after HR treatment without corrosion (g) and after corrosion (h, i) (Arrows in Fig.5h point to the spherical precipitates)
Fig.6  Composition analyes of precipitates formed in Fe-0.03C-10Cr-0.2Zr-0.3V steel aged at 700oC for 1000 h after HR + N treatment by EDS analysis (a) and Thermo-Calc prediction (b)
MethodAtomic fractionMass fraction
ZrNbCZrNbC
TEM-EDS analysis0.460.140.400.710.210.08
Thermo-Calc prediction0.420.0930.490.7230.1650.112
Table 1  Chemical composition of precipitates formed in Fe-0.03C-10Cr-0.2Zr-0.3V steel aged at 700oC for 1000 h after HR + N treatment
Fig.7  HRTEM image (a), and FFT (b) and IFFT (c) diagrams of precipitate formed in Fe-0.03C-10Cr-0.2Zr-0.3V steel aged at 700oC for 1000 h after HR + N treatment
Fig.8  High-temperature Vickers hardnesses of Fe-0.03C-10Cr-0.2Zr-0.3V steel tested at 700oC
Fig.9  Creep properties of Fe-0.03C-10Cr-0.2Zr-0.3V steel tested at 650oC (a, c) and 700oC (b, d) (σth—threshold stress)
(a, b) minimum creep rate vs applied stress (c, d) (creep rate)1/4vs applied stress
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