真空热处理对8% Y2O3+ZrO2涂层在LiCl-KCl熔盐中的耐腐蚀行为的影响

冯力; 唐恒; 崔军鹏; 马超; 成波

doi:10.16490/j.cnki.issn.1001-3660.2026.20.004

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表面技术 ›› 2026, Vol. 55 ›› Issue (20) : 41-54. DOI: 10.16490/j.cnki.issn.1001-3660.2026.20.004

腐蚀与防护

真空热处理对8% Y₂O₃+ZrO₂涂层在LiCl-KCl熔盐中的耐腐蚀行为的影响

冯力^1a,b*, 唐恒^1a, 崔军鹏^1a, 马超^1a,3, 成波^1b

作者信息 +

Effect of Vacuum Heat Treatment on the Corrosion Resistance Behavior of 8wt.% Y₂O₃+ZrO₂ Coating in LiCl-KCl Molten Salt

FENG Li^1a,b*, TANG Heng^1a, CUI Junpeng^1a, MA Chao^1a,3, CHENG Bo^1b

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摘要

目的强化大气等离子喷涂8% Y₂O₃+ZrO₂（8YSZ）涂层在电解精炼槽LiCl-KCl高温熔盐环境中的服役性能,延长涂层的服役寿命。方法本研究采用大气等离子喷涂技术在316L不锈钢基体表面制备8YSZ涂层,并对其进行不同参数的真空热处理（700 ℃-2 h、900 ℃-1 h、900 ℃-2 h、900 ℃-3 h和1 100 ℃-2 h）,研究其在LiCl-KCl高温熔盐环境中的耐腐蚀性能,采用装备能谱仪的扫描电子显微镜（SEM+EDS）、X射线衍射（XRD）和X射线光电子能谱（XPS）等手段表征热处理前后涂层的微观形貌、元素分布和物相组成。结果热处理技术显著提升了涂层的致密性,其中涂层经900 ℃-2 h热处理后孔隙率最低,为5.81%,相较于未热处理的涂层孔隙率降低了42.98%。未经热处理的涂层在腐蚀320 h后出现了明显的涂层脱落现象,而经过真空热处理后的样品在经过320 h腐蚀后涂层依然保持结构完整。结论真空热处理通过促进涂层致密化,有效抑制了高温熔盐沿孔隙向涂层内的快速渗透,延缓了腐蚀介质的输运过程与腐蚀反应的发生,从而延长了8YSZ涂层在LiCl-KCl高温熔盐环境中的服役寿命。

Abstract

Atmospheric plasma-sprayed 8wt.% yttria-stabilized zirconia (8YSZ) coatings have been widely used for structural protection in high-temperature molten salt environments, such as electrorefining cells, owing to their excellent thermal stability and low thermal conductivity. However, during long-term service, LiCl-KCl molten salt can readily penetrate the inherent pores and microcracks of plasma-sprayed coatings, leading to coating spallation and premature failure, which seriously threatens the service life and operational reliability of electrorefining cells and related structural components. To address this issue, 8YSZ coatings were prepared on 316L stainless steel substrates by atmospheric plasma spraying (APS), and the effects of different vacuum heat-treatment schedules on their microstructural evolution and corrosion behavior in LiCl-KCl molten salt were systematically investigated. Scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were employed to characterize the microstructure, elemental distribution, phase composition, and surface chemical states of the coatings. The results showed that vacuum heat treatment significantly promoted the sintering densification of the 8YSZ coating. The as-sprayed coating exhibited a typical APS lamellar structure with numerous irregular pores, microcracks, and partially unmelted particles, and its porosity was approximately 10.19%. After heat treatment, the coating became progressively denser. In particular, the coating heat-treated at 900 ℃ for 2 h showed the most pronounced densification effect, with the porosity decreasing from 10.19% to 5.81%, corresponding to a reduction of 42.98%. SEM observations indicated that some interconnected pores gradually shrank, spheroidized, or became partially closed during heat treatment. EDS mapping further suggested that vacuum heat treatment promoted limited elemental redistribution near the coating interface. The as-sprayed coating and the optimally heat-treated coating were then subjected to isothermal corrosion tests in LiCl-KCl molten salt at 600 ℃ for up to 320 h. After 320 h of exposure, the as-sprayed coating exhibited obvious local spallation. Cross-sectional SEM and EDS analyses revealed that molten salt penetrated rapidly through interconnected pores and cracks toward the coating/substrate interface, where corrosion products containing Cl and O were detected. In contrast, the coating heat-treated at 900 ℃ for 2 h remained structurally intact under the same corrosion conditions. The cross-sectional observations confirmed that the main body of the heat-treated coating retained a relatively dense structure, maintained good adhesion to the substrate, and showed no obvious spallation. The improved corrosion resistance of the heat-treated coating can be mainly attributed to the enhanced physical barrier effect induced by sintering densification. The denser coating structure effectively blocked fast penetration channels for molten salt, prolonged the diffusion path of corrosive species, and delayed interfacial corrosion reactions. In addition, XRD results showed that no additional crystalline phases were detected after corrosion, indicating that the 8YSZ coating maintained good phase stability in the LiCl-KCl molten salt environment. Overall, vacuum heat treatment at 900 ℃ for 2 h effectively enhanced the corrosion resistance of the APS 8YSZ coating by reducing connected defects and suppressing molten salt penetration. This work provides a feasible post-treatment strategy for improving the durability of protective ceramic coatings used in electrorefining cells and other high-temperature molten salt environments.

导出引用

冯力, 唐恒, 崔军鹏, 马超, 成波. 真空热处理对8% Y₂O₃+ZrO₂涂层在LiCl-KCl熔盐中的耐腐蚀行为的影响[J]. 表面技术. 2026, 55(20): 41-54

FENG Li, TANG Heng, CUI Junpeng, MA Chao, CHENG Bo. Effect of Vacuum Heat Treatment on the Corrosion Resistance Behavior of 8wt.% Y₂O₃+ZrO₂ Coating in LiCl-KCl Molten Salt[J]. Surface Technology. 2026, 55(20): 41-54

中图分类号： TG174

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