Effect of Si on Microstructure and Mechanical Properties of a 9Cr Ferritic/Martensitic Steel
ZHANG Qiankun1,2, HU Xiaofeng1(), JIANG Haichang1, RONG Lijian1
1.CAS Key Laboratory of Nuclear Materials and Safety Assessment, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China 2.School of Materials Science and Engineering, University of Science and Technology of China, Shenyang 110016, China
Cite this article:
ZHANG Qiankun, HU Xiaofeng, JIANG Haichang, RONG Lijian. Effect of Si on Microstructure and Mechanical Properties of a 9Cr Ferritic/Martensitic Steel. Acta Metall Sin, 2024, 60(9): 1200-1212.
Due to the worsening of environmental pollution and energy shortage, nuclear energy has become an increasingly important energy source, offering clean, high-energy, safe, and stable power to meet the needs of modern life and production. P91 steel is an excellent heat-resistant steel, widely used in nuclear power plants for its good mechanical properties, high thermal conductivity, and low irradiation swelling rate. However, with the emergence of lead and lead-bismuth eutectic (LBE) cooled fast reactors (LFRs), P91 steel's inferior compatibility with LBE has limited its use in LFR construction. To address this issue, 9Cr ferritic/martensitic steel with high Si content (H-Si steel) was designed in this study to develop a compatible structural material for LFR heat exchange tubes. In addition, the effects of Si on the microstructure and mechanical properties of as-cast, homogenized, tempered, and aged H-Si steel were investigated using various techniques, including OM, FESEM, TEM, EBSD, tensile, and impact tests. The results show that the increase in Si content leads to 3.9% δ ferrite (volume fraction) in as-cast H-Si steel, which can be eliminated completely by homogenization heat treatment. Tempering produces a Si-enriched layer around M23C6 due to the high Si content in the H-Si steel, which can suppress the rapid growth of M23C6 and maintain a smaller size of M23C6 than that of M23C6 in P91 steel. Meanwhile, the Si-enriched layer can slow down the growth of M23C6 and promote the nucleation and growth of the Laves phase during aging at 550°C, which induces smaller M23C6 and larger Laves phase in aged H-Si steel than that in aged P91. Due to the higher Si content and smaller M23C6, the tempered H-Si steel exhibits significantly higher strength than P91. After aging, the strength of H-Si steel further increases because of the precipitation of the Laves phase. Both tempered alloy steels have similar impact energy (about 210 J) and the fracture mode is ductile fracture. However, the precipitation of the Laves phase after aging decreases the impact energy of both alloy steels. The aged H-Si steel had a larger and more Laves phase, resulting in a partial cleavage area in the impact fracture surface and inducing a lower impact energy compared to H-Si steel.
Fund: LingChuang Research Project of China National Nuclear Corporation, Youth Innovation Promotion Association CAS(Y2021059);Strategic Priority Research Program of the Chinese Academy of Sciences(XDA28040200)
Corresponding Authors:
HU Xiaofeng, professor, Tel: (024)23971981, E-mail: xfhu@imr.ac.cn
Table 1 Tensile properties and impact energies at room temperature for P91 and H-Si alloy steels at tempered and aged states
Fig.1 OM images of as-cast P91 (a) and H-Si (b) steels and homogenized H-Si steel (c)
Fig.2 OM images of tempered P91 (a) and H-Si (b) steels
Fig.3 SEM images of tempered P91 (a, c) and H-Si (b, d) steels at lower (a, b) and higher (c, d) magnifications, and the EDS analyses (e, f) of particles A (e) and B (f) in tempered P91 steel as shown in Fig.3c
Fig.4 TEM images of tempered P91 (a) and H-Si (b) steels (Insets in Fig.4b show the selected area electron diffraction (SAED) patterns of particles C and D )
Fig.5 SEM images of aged P91 (a, c) and H-Si (b, d) steels at lower (a, b) and higher (c, d) magnifications
Fig.6 TEM image of aged P91 (a) and H-Si (b) steels and the elements mapping of the area denoted by the rectangle in Fig.6b (c) (Inset in Fig.6b is the SAED pattern of particle E)
Fig.7 EBSD phase distribution images of aged P91 (a) and H-Si (b) steels
Fig.8 Changes of phase transition temperature of P91 and H-Si alloy steels
Precipitate
Tempered state
Aged state
P91
H-Si
P91
H-Si
M23C6
106 ± 35
82 ± 32
135 ± 38
98 ± 38
NbC
515 ± 12
512 ± 14
512 ± 14
514 ± 21
Laves phase
-
-
79 ± 32
129 ± 47
Table 2 Precipitate sizes of P91 and H-Si alloy steels at tempered and aged states
Fig.9 TEM image of M23C6 precipitated at boundaries of tempered H-Si steel (a), elements mapping image of the area denoted by the rectangle in Fig.9a (b), and line scanning image of M23C6 along the line in Fig.9b (c)
Fig.10 TEM image of M23C6precipitated at boundaries of tempered P91 steel (a) and elements mapp-ing image of the area denoted by the rectangle in Fig.10a (b)
Fig.11 SEM images of impact fracture surfaces of aged P91 (a) and H-Si (b) steels at room temperature (Inset in Fig.11b is the magnified image of the rectangle area, and dotted line shows the cleavage zone)
Fig.12 Cross section SEM images of aged P91 (a) and H-Si (b) steels near the impact fracture surfaces (Inset in Fig.12b is the EBSD phase distribution image of the impact fracture surface denoted by rectangle)
1
Bassini S, Cataldo S, Cristalli C, et al. Material performance in lead and lead-bismuth alloy [J]. Compr. Nucl. Mater., 2020, 4: 218
2
Cabet C, Dalle F, Gaganidze E, et al. Ferritic-martensitic steels for fission and fusion applications [J]. J. Nucl. Mater., 2019, 523: 510
doi: 10.1016/j.jnucmat.2019.05.058
3
Gong X, Short M P, Auger T, et al. Environmental degradation of structural materials in liquid lead- and lead-bismuth eutectic-cooled reactors [J]. Prog. Mater. Sci., 2022, 126: 100920
4
Alemberti A. The lead fast reactor: An opportunity for the future? [J]. Engineering, 2016, 2: 59
5
Yang K, Yan W, Wang Z G, et al. Development of a novel structural material (SIMP steel) for nuclear equipment with balanced resistances to high temperature, radiation and liquid metal corrosion [J]. Acta Metall. Sin., 2016, 52: 1207
Martinelli L, Balbaud-Célérier F, Terlain A, et al. Oxidation mechanism of a Fe-9Cr-1Mo steel by liquid Pb-Bi eutectic alloy (Part I) [J]. Corros. Sci., 2008, 50: 2523
7
Martinelli L, Balbaud-Célérier F, Picard G, et al. Oxidation mechanism of a Fe-9Cr-1Mo steel by liquid Pb-Bi eutectic alloy (Part III) [J]. Corros. Sci., 2008, 50: 2549
8
Martinelli L, Balbaud-Célérier F, Terlain A, et al. Oxidation mechanism of an Fe-9Cr-1Mo steel by liquid Pb-Bi eutectic alloy at 470°C (Part II) [J]. Corros. Sci., 2008, 50: 2537
9
Wang J, Lu S P, Rong L J, et al. Effect of silicon on the oxidation resistance of 9wt.% Cr heat resistance steels in 550oC lead-bismuth eutectic [J]. Corros. Sci., 2016, 111: 13
10
Chen S H, Rong L J. Effect of silicon on the microstructure and mechanical properties of reduced activation ferritic/martensitic steel [J]. J. Nucl. Mater., 2015, 459: 13
11
Zhang Y Y, He H, Wang H, et al. Evolution of microstructure and mechanical properties of 9Cr ferrite/martensite steels with different Si content after long-term aging at 550oC [J]. J. Alloys Compd., 2021, 873: 159817
12
Zhou J, Qiu S Y, Qiu R S, et al. Effect of Si content on precipitation behavior of Laves phase and impact performance of 9%Cr ferritic martensitic steel [J]. Trans. Mater. Heat Treat., 2022, 43(5): 116
Ryu S H, Yu J. A new equation for the Cr equivalent in 9 to 12 pct Cr steels [J]. Metall. Mater. Trans., 1998, 26A: 1573
14
Liu Z, Liu Z D, Wang X T, et al. Investigation of the microstructure and strength in G115 steel with the different concentration of tungsten during creep test [J]. Mater. Charact., 2019, 149: 95
15
Tan L, Yang Y, Busby J T. Effects of alloying elements and thermomechanical treatment on 9Cr reduced activation ferritic-martensitic (RAFM) steels [J]. J. Nucl. Mater., 2013, 442: S13
16
Ye Z F, Wang P, Li D Z, et al. Effect of carbon and niobium on the microstructure and impact toughness of a high silicon 12% Cr ferritic/martensitic heat resistant steel [J]. Mater. Sci. Eng., 2014, A616: 12
17
Chen F X. Study on the microstructural evolution and strength degradation of 9% chromium ferritic/martensitic heat resistant steels [D]. Zibo: Shandong University of Technology, 2009
Zhang Y, Yu C, Zhou T, et al. Effects of Ti and a twice-quenching treatment on the microstructure and ductile brittle transition temperature of 9CrWVTiN steels [J]. Mater. Des., 2015, 88: 675
19
Yin H F, Yang G, Zhao J Q, et al. Mo-rich Laves phase in a 9.5Cr-1.5MoCoVNbNB heat-resistant steel during long-term aging at 620oC [J]. Mater. Charact., 2021, 182: 111588
20
Isik M I, Kostka A, Yardley V A, et al. The nucleation of Mo-rich Laves phase particles adjacent to M23C6 micrograin boundary carbides in 12% Cr tempered martensite ferritic steels [J]. Acta Mater., 2015, 90: 94
21
Isik M I, Kostka A, Eggeler G. On the nucleation of Laves phase particles during high-temperature exposure and creep of tempered martensite ferritic steels [J]. Acta Mater., 2014, 81: 230
22
Wang X, Yu S M, Ren Y Y, et al. Laves phase evolution in P92 steel during ageing [J]. Acta Metall. Sin., 2014, 50: 1195
doi: 10.11900/0412.1961.2014.00101
Aghajani A, Somsen C, Eggeler G. On the effect of long-term creep on the microstructure of a 12% chromium tempered martensite ferritic steel [J]. Acta Mater., 2009, 57: 5093
24
Xue W Y, Zhou J H, Shen Y F, et al. Micromechanical behavior of a fine-grained China low activation martensitic (CLAM) steel [J]. J. Mater. Sci. Technol., 2019, 35: 1869
doi: doi.org/10.1016/j.jmst.2019.05.005
25
Xu Y T, Nie Y H, Wang M J, et al. The effect of microstructure evolution on the mechanical properties of martensite ferritic steel during long-term aging [J]. Acta Mater., 2017, 131: 110
26
Li J R, He T, Zhang P F, et al. Effect of large-size carbides on the anisotropy of mechanical properties in 11Cr-3Co-3W martensitic heat-resistant steel for turbine high temperature blades in ultra-supercritical power plants [J]. Mater. Charact., 2020, 159: 110025
27
Yan P, Liu Z D. Toughness evolution of 9Cr-3W-3Co martensitic heat resistant steel during long time aging [J]. Mater. Sci. Eng., 2016, A650: 290
28
Lee J S, Armaki H G, Maruyama K, et al. Causes of breakdown of creep strength in 9Cr-1.8W-0.5Mo-VNb steel [J]. Mater. Sci. Eng., 2006, A428: 270