基于熔盐电解法的乏燃料干法后处理技术是实现我国核燃料闭式循环的关键步骤。在熔盐电解过程中，以碱金属的混合氯盐为溶剂，在500-600℃高温条件下，经电解提取、精炼、蒸馏等一系列工艺，从乏燃料中高效分离回收铀、钚及其他有价值的核素。然而，这一过程也带来了严峻的挑战：相关设备长期暴露于高温氯化物熔盐环境，服役材料面临着严重的高温腐蚀问题。因此，为了进一步提升服役材料在熔盐腐蚀环境中的服役性能，亟待探索一种经济有效的高温防护方案，早日实现核燃料闭式循环。
         晶界工程（Grain Boundary Engineering，GBE）是一种先进的材料改性技术，通过调控材料内部的晶界结构，优化材料的综合性能。本试验以核用GH3535合金为研究材料，采用晶界工程优化该合金的组织结构，对比研究固溶态与晶界工程态的GH3535合金在氯化物熔盐环境中的腐蚀性能和高温力学性能，旨在提供一种简单易行的材料改性方案，提升合金材料在氯化物熔盐环境下的服役性能。研究结果显示，在550℃氩气保护的45LiCl-55KCl wt.%熔盐环境中，经过300 h的腐蚀试验后，固溶态（Non-GBE）试样表面形成了由非连续富Cr外氧化层、去合金化Ni₃Fe层和内氧化NiCr₂O₄层构成的三层结构，腐蚀程度较为严重。相比之下，晶界工程态（GBE-2）试样的腐蚀程度极为轻微，表面未出现明显的腐蚀退化现象。在熔盐腐蚀后，Non-GBE试样的高温延伸率显著降低，脆性腐蚀产物层以及优先被腐蚀的随机晶界加剧了裂纹的萌生与扩展。而GBE试样的高温力学性能并未出现退化现象，其高密度孪晶界与时效析出的晶内碳化物共同保障了合金在变形过程中的稳定动态应变时效（DSA）性能，在耐蚀性和高温力学性能方面表现突出。对比之下，发现熔盐蒸气腐蚀和熔盐液态腐蚀原理一致，但腐蚀程度更为严重。

         尽管晶界工程对GH3535合金的性能有所提升，但在熔盐蒸气环境下，合金的腐蚀问题依然严峻。因此，高效的高温防护措施成为当务之急。本文设计单一/多元氮化物涂层和基于SiO₂-B₂O₃-Na₂O-CaO氧化物相的搪瓷涂层作为乏燃料熔盐电解结构材料的防护材料。在550℃下的LiCl-KCl气氛中，对氮化物涂层涂覆搪瓷涂层的GH3535合金进行了腐蚀行为研究。结果表明，氮化物涂层在熔盐腐蚀下完全失效。搪瓷涂层为非晶态，与合金基体紧密结合。腐蚀动力学分析表明，搪瓷涂层的质量损失远低于GH3535合金，表明搪瓷涂层在氯化物盐中具有较高的化学稳定性和较低的孔隙率，可以有效地阻断Cl^-向搪瓷涂层/合金界面的扩散。经过300 h腐蚀试验后，搪瓷涂层表面虽有腐蚀产物生成，但在长时间的实验中未出现开裂或剥落行为，熔盐也未渗入涂层内部。

     The dry reprocessing technology of spent fuel based on molten salt electrolysis is the key step to realize the closed cycle of nuclear fuel in China. the process of molten salt electrolysis, the mixed chloride of alkali metal is used as solvent, and a series of processes such as extraction, refining and distillation are out at high temperature of 500-600℃ to efficiently separate and recover uranium, plutonium and other valuable nuclear species from spent fuel. However, this also brings serious challenges: the relevant equipment is exposed to the high-temperature chloride molten salt environment for a long time, and the service materials are facing serious high-temperature problems. Therefore, in order to further improve the service performance of service materials in molten salt corrosion environment, it is urgent to explore an economical and effective high-temperature protection scheme achieve the closed cycle of nuclear fuel as soon as possible.

     Grain Boundary Engineering (GBE) is an advanced material modification technology that optimizes the comprehensive performance of materials by regulating the grain structure within the material. In this study, nuclear-grade GH3535 alloy was used as the research material. The microstructure of the alloy was optimized using grain boundary, and the corrosion performance and high-temperature mechanical properties of the GH3535 alloy in a chloride molten salt environment were compared between the solid-solution state and grain boundary engineering state. The aim was to provide a simple and feasible material modification scheme to improve the service performance of alloy materials in a chloride molten salt environment. The showed that after 300 h of corrosion test in an argon-protected 45LiCl-55KCl wt.% molten salt environment at 50℃, the surface of the solid-solution (Non-GBE) sample formed a three-layer structure consisting of a discontinuous rich-Cr outer oxide layer, dealloyed Ni₃Fe layer, and an inner oxidized NiCr₂O₄ layer, with a relatively serious degree of corrosion. In contrast, the corrosion degree of grain boundary engineering (GBE-2) sample was extremely slight, and no significant corrosion degradation phenomenon was observed on the surface. After molten salt corrosion, the high-temperatureation of the Non-GBE sample decreased significantly, and the brittle corrosion product layer and the preferentially corroded random grain boundaries aggravated the initiation and expansion of. In contrast, the high-temperature mechanical properties of the GBE sample did not show any degradation phenomenon, and its high-density twin boundaries and aging precipitated intragranularides together ensured the stable dynamic strain aging (DSA) performance of the alloy during deformation, showing excellent performance in corrosion resistance and high-temperature mechanical properties. In comparison, it found that the principle of molten salt vapor corrosion and molten salt liquid corrosion is consistent, but the degree of corrosion is more serious.

     Although grain boundary engineering has improved the properties of GH3535 alloy, the corrosion problem of the alloy still needs to be addressed the molten salt vapor environment. Therefore, efficient high-temperature protection measures have become an urgent task. In view of the shortcomings of traditional ceramic coatings, this paper designs singlemultiple nitride coatings and enamel coatings based on SiO₂-B₂O₃-Na₂O-CaO oxide phases as protective materials for the structure materials spent fuel molten salt electrolysis. The corrosion behavior of GH3535 alloy with nitride coating coated with enamel coating was investigated in a LiCl-KCl at 550℃. The results show that the nitride coating fails completely under molten salt corrosion. The enamel coating is amorphous and closely bonded to the substrate. Corrosion kinetics analysis shows that the mass loss of the enamel coating is far less than that of GH3535 alloy, indicating that the en coating has high chemical stability and low porosity in chloride salts and can effectively block the diffusion of Cl^- to the enamel coating/alloy interface. After 300 h of corrosion test, although corrosion products are generated on the surface of the enamel coating, no cracking or peeling behavior is observed during the long-term experiment, and theten salt does not penetrate into the interior of the coating.

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