Early corrosion behavior of high Si austenitic stainless steel in oxygen-saturated lead-bismuth eutectic (LBE) at 550 °C

doi:10.1016/j.metadv.2026.03.003

Abstract

Abstract:

The oxide film formed on Fe-15Cr-9Ni-2.5Si austenitic stainless steel exposed to oxygen-saturated static lead-bismuth eutectic (LBE) at 550 °C for 1-50 h has been investigated by multiscale characterization methods such as scanning electron microscope (SEM) and transmission electron microscopy (TEM). The results reveal that the oxide film formed at the early stage of corrosion has a multi-layer structure. The thickness of the oxide film increases linearly and the stratification of the oxide film becomes more pronounced with the extension of time. The outer oxide film is composed of magnetite and plumboferrite, and the loose porous plumboferrite promotes LBE penetration resulting in reduced protection of the outer oxide film. The inner oxide film is composed of an extremely thin (Cr, Si)-rich oxide film, a Ni-depleted spinel layer and a dual-phase network structure composed of (Fe, Ni) phase and spinel. The high Si content leads to the preferential formation of a thin (Cr, Si)-rich oxide film at the interface and the formation of Si-rich spinel inner oxide film, which suppress the dissolution and diffusion of elements and improve the oxidation resistance of the inner oxide film. The early corrosion mechanism of austenitic stainless steel in liquid LBE is discussed.

Key words: Lead-bismuth eutectic, Austenitic stainless steel, Oxidation, (Cr, Si)-rich oxide film, Transmission electron microscopy (TEM)

Xiaoqi Geng, Yongxin Cheng, Neng He, Ang Xie, Tingting Yao, Shenghu Chen, Cuihong Li, Zhaodong Wang, Chunlin Chen, Lijian Rong. Early corrosion behavior of high Si austenitic stainless steel in oxygen-saturated lead-bismuth eutectic (LBE) at 550 °C[J]. Metals Advances, 2026, 47: 88-100.

Figures/Tables 17

Fig. 1. EBSD and TEM results of Fe-15Cr-9Ni-2.5Si steel: (a) band contrast map; (b) phase map; (c) high resolution TEM (HRTEM) image; (d) grain size distribution image; (e) inverse pole figure (IPF) map; (f) SAED pattern.

Fig. 2. XRD patterns of Fe-15Cr-9Ni-2.5Si steel exposed to oxygen-saturated liquid LBE at 550 °C for 1 h, 10 h, and 50 h.

Fig. 3. SEM images of surface oxides exposed to oxygen-saturated liquid LBE at 550 °C for 1 h (a, d), 10 h (b, e), and 50 h (c, f).

Table 1. Chemical composition of oxides formed on the surface exposed to oxygen-saturated liquid LBE at 550 °C for 1 h, 10 h, and 50 h (in wt%).

Position	Pb	Bi	O	Fe	Cr	Ni
A	18.28	42.69	9.45	20.60	−	−
B	−	−	−	70.59	14.83	8.96
C	54.48	−	15.21	17.74	−	−
D	30.21	−	26.91	37.86	−	−

Fig. 4. BSE images of cross-section of oxide films exposed to oxygen-saturated liquid LBE at 550 °C for 1 h (a, b), 10 h (c), and 50 h (d).

Fig. 5. EPMA images of cross-section of oxide films exposed to oxygen-saturated liquid LBE at 550 °C for 1 h (a), 10 h (b), and 50 h (c).

Fig. 6. Variations in thickness of oxide film as a function of time after exposure to oxygen-saturated static LBE at 550 °C.

Fig. 7. HAADF images of cross-section of oxide films exposed to oxygen-saturated liquid LBE at 550 °C for 1 h (a, b), 10 h (c), and 50 h (d).

Fig. 8. HAADF image and maps revealing Pb, Bi, O, Fe, Cr, Ni and Si distributions of inner oxide film exposed to oxygen-saturated liquid LBE at 550 °C for 1 h.

Fig. 9. TEM results of inner oxide film exposed to oxygen-saturated liquid LBE at 550 °C for 1 h: (a) HAADF image and maps revealing Fe, O, Si, Cr, and Ni distributions; (b-d) SAED patterns corresponding to the white rectangular areas in (a).

Fig. 10. TEM images of outer oxide film exposed to oxygen-saturated liquid LBE at 550 °C for 1 h: (a) TEM image; (b, d) TEM image corresponding to the white rectangular areas in (a); (c, e) SAED patterns corresponding to the area in (b, d).

Fig. 11. TEM images of outer oxide film exposed to oxygen-saturated liquid LBE at 550 °C for 50 h: (a) TEM image; (b, d) HRTEM images corresponding to the white rectangular areas in (a); (c, e) SAED patterns corresponding to the area in (b, d).

Fig. 12. TEM results of inner oxide film exposed to oxygen-saturated liquid LBE at 550 °C for 50 h: (a) HAADF image; (b) maps revealing Fe, O, Cr, and Ni distributions corresponding to the red rectangular area in (a); (c-e) SAED patterns corresponding to the red rectangular areas in (a).

Fig. 13. STEM images of the dual-phase structure in inner oxide film exposed to oxygen-saturated liquid LBE at 550 °C for 50 h: (a) HAADF image and maps revealing Fe, O, Si, Cr, and Ni distributions; (b) STEM-EDS line scan across the dual-phase structure.

Fig. 14. TEM results of the inner/outer oxide film interface exposed to oxygen-saturated liquid LBE at 550 °C for 50 h: (a) HAADF image and maps revealing Fe, O, Si, Cr, and Ni distributions of the interface; (b) TEM image; (c, d) HRTEM images corresponding to the white rectangular areas in (b); (c1-d1) FFT patterns corresponding to the area in (c, d).

Fig. 15. TEM results of the oxidation front in inner oxide film exposed to oxygen-saturated liquid LBE at 550 °C for 50 h: (a) TEM image; (b, c) HRTEM images corresponding to the white rectangular areas in (a); (b1-c1) FFT patterns corresponding to the area in (b, c); (d) HAADF image corresponding to the red rectangular areas in (a) and maps revealing Fe, O, Cr, and Ni distributions; (e) EDS line scan across the dual-phase structure.

Fig. 16. Schematic illustration of the corrosion process of Fe-15Cr-9Ni-2.5Si austenitic stainless steel in oxygen-saturated liquid LBE at 550 °C: (a, b) 1 h; (c) 10 h; (d) 50 h.

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