采用原位氧化的方法,通过氢化锆直接与02反应在表面生成氧化膜作为氢渗透阻挡层。分析了氧化工艺参数对氧化膜生长速度的影响,并对氧化膜的物相组成、截面形貌和阻氢性能进行了研究。结果表明,温度是影响氧化膜生长速度的主要因素,氢化锆在450℃以下的温度范围内氧化,氧化膜生长速度很小,氧气分压对氧化膜生长速度无明显影响;在450℃以上,氧化膜生长速度随着氧气分压的增大和氧化温度的升高而增大;氧化膜的质量增重与氧化时间的关系曲线符合抛物线生长规律。氧化膜为双相复合结构,由单斜相M—ZrO2和四方相T—ZrO2组成。氢化锆原位氧化后经650℃真空脱氢50h后样品失氢量低于0.2%。
Hydrogen permeation barrier on the surface of zirconium hydride was prepared by oxidation in situ. The influences of oxidation parameters on the mass gain percentage of oxide film were investigated. The morphology, phase structure and damp property of oxide film were analyzed. The results indicated that oxidation temperature had a great influence on oxidation rate. The growth speed of oxide film was slow when oxidation temperature was below 450 ~C. The partial oxygen pressure had little effect on oxidation rate. The growth speed of oxide film increased with the increase of partial oxygen pressure and oxidation temperature. A parabolic law was observed in the curves of mass gain of the oxide film with oxidation time increasing. The main phase of oxide film was mono- clinic and tetragonal ZrO2. Hydrogen lose of zirconium hydride with oxide film was below 0.2% in dehydrogenation processes at 650 ℃ for 50 h.