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采用溶胶-凝胶法制备锆的醇盐,以锆的醇盐为前驱体涂在氢化锆表面制备氧化锆膜层以防止氢化锆中氢析出。研究了热处理温度对氧化锆膜层的物相组成、形貌及阻氢性能的影响。利用扫描电子显微镜(SEM)、激光共聚焦显微镜(CLSM)、X射线衍射仪(XRD)分析测试了氧化锆膜层的截面形貌、表面形貌及相结构。通过真空脱氢实验对膜层的阻氢性能进行评估。结果表明,热处理温度在600℃以上时,可以在氢化锆表面获得致密并连续的氧化锆膜层;氧化锆膜层的阻氢因子PRF(permeation reduction factor)值随着热处理温度的升高呈现出先增大后减小的趋势,当热处理温度为600℃时获得氧化锆膜层的阻氢因子最高,为8.6;氧化锆膜层主要由四方相氧化锆T-ZrO_2和单斜相氧化锆M-ZrO_2组成,并以单斜相氧化锆M-ZrO_2为主。
A zirconium alkoxide was prepared by a sol-gel method. The zirconium alkoxide was used as a precursor to prepare a zirconium oxide film on the surface of the zirconium hydride to prevent the hydrogen in the zirconium hydride from precipitating. The effects of heat treatment temperature on the phase composition, morphology and hydrogen storage properties of zirconia films were investigated. The morphology, morphology and phase structure of the zirconia film were investigated by scanning electron microscopy (SEM), confocal laser scanning microscopy (CLSM) and X-ray diffraction (XRD) The hydrogen barrier properties of the films were evaluated by vacuum dehydrogenation experiments. The results show that the dense and continuous ZrO2 film can be obtained on the surface of ZrO2 when the temperature is above 600 ℃. The value of PRF (permeation reduction factor) of zirconium oxide film increases with the increase of heat treatment temperature And then decreased. When the heat treatment temperature was 600 ℃, the highest hydrogen evolution factor was obtained for the zirconium oxide film, which was 8.6. The zirconium oxide film was mainly composed of tetragonal zirconia T-ZrO 2 and monoclinic zirconia M- ZrO 2 and monoclinic zirconia M-ZrO 2.