采用溶胶凝胶技术,以氧氯化锆/乙醇/水为反应体系在氢化锆表面制备氧化锆膜层作为防氢渗透层,研究了溶胶pH值对氧化锆膜层的物相组成、截面形貌及阻氢性能的影响。利用涡流测厚仪、扫描电子显微镜(SEM)、x射线衍射仪(XRD)分析测试了氧化锆膜层的厚度、截面形貌及相结构。通过真空脱氢实验测试评估膜层的阻氢性能。结果表明,在选取的溶胶pH值为1—9范围内,膜层的厚度在7.6~14.8μm之间变化,膜层的氢渗透降低因子(PRF)值在9.8~11.5之间变化,膜层厚度和膜层的氢渗透降低因子(PRF)值都随着pH值增大呈现出先增加后减小的变化趋势。当pH为5时,膜层厚度达到最大值14.8μm,膜层的PRF值达到11.5,膜层与基体结合紧密,膜层连续完整、致密均匀。pH值变化对膜层物相组成没有显著影响,膜层由单斜相M—ZrO1.8和四方相T—ZrO1.8组成,其中以单斜相M-ZrO1.8为主。
Zirconium oxide films were prepared on the surface of zirconium hydride as preventing hydrogen permeability layers by sol- gel method in the reaction system of oxygen zirconium chloride ethanol in water. The thickness, cross-sectional morphologies and struc- ture of the oxide films were characterized by thickness gauge, scanning election microscopy(SEM) and X-ray diffraction( XRD), re- speetively. Hydrogen resistance performance was evaluated by the method of vacuum dehydrogenation. The results showed that the thickness of oxide films varied from 7.6 to 14.8 μm and permeation reduction factor(PRF) varied from 9.8 to 11.5 μm. The thick- ness and PRF values of oxide films presented an initial increase and then a decrease during the pH increseent process. The maximum thickness of oxide films was 14.8 and the maximum PRF of oxide films was 11.5 when the pH was 5. The continuous uniform zirconium oxide films could be gained while zirconium oxide film and zirconium hydride substrate were tightly bounded. The phase structure of oxide films was composed of monoclinic ZrO1.8 and tetragonal ZrO1.8 with different pH values, but monoclinie ZrO1.8 was the main phase.