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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 film was prepared on the surface of zirconium hydride by using zirconium oxychloride / ethanol / water as the hydrogen permeation barrier by sol-gel technique. The effects of sol pH on the phase composition, cross-section Appearance and hydrogen barrier properties. The thickness, cross-sectional morphology and phase structure of the zirconia film were measured by eddy current thickness measurement, scanning electron microscopy (SEM) and X-ray diffraction (XRD) The hydrogen barrier property of the film was evaluated by vacuum dehydrogenation test. The results show that the film thickness varies from 7.6 to 14.8μm at the pH range of 1 to 9, and the hydrogen permeation reduction factor (PRF) of the film varies from 9.8 to 11.5. The film thickness Both the thickness and the hydrogen permeation reduction factor (PRF) value of the membrane showed a trend of first increasing and then decreasing with the increase of pH value. When the pH is 5, the film thickness reaches the maximum of 14.8μm, the PRF value of the film reaches 11.5, and the film layer is tightly combined with the substrate. The film layer is continuous and compact and uniform. The change of pH value had no significant effect on the phase composition of the coating. The film consisted of monoclinic phase M-ZrO1.8 and tetragonal phase T-ZrO1.8, of which monoclinic phase M-ZrO1.8 was the dominant one.