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采用溶胶凝胶技术,以正丙醇锆为前驱体,在氢化锆表面制备氧化锆防氢渗透层。研究了当热处理温度为600℃时,不同热处理气氛对溶胶凝胶法制备的氧化锆膜层的截面形貌、表面形貌、物相组成以及阻氢性能的影响。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)和涡流测厚仪分别测试了氧化锆膜层的截面形貌、表面形貌、相结构及厚度。利用真空脱氢实验对膜层的阻氢性能进行评估。研究结果表明,当热处理气氛中有氧存在时,可在氢化锆表面制得连续、致密的氧化锆膜层;而当热处理气氛中无氧存在时,所制备的氧化锆膜层不连续、均匀性差。热处理气氛中有氧时制备的氧化锆膜层的阻氢效果较无氧时要好,膜层厚度为10.1μm,渗透降低因子(PRF)值为8.4。而不同热处理气氛对氧化锆膜层的物相组成没有显著影响,膜层主要由单斜相氧化锆M-ZrO_2和四方相氧化锆TZrO_2组成,并以单斜相氧化锆M-ZrO_2为主。
The sol-gel technique was used to prepare the zirconia hydrogen permeation layer on the surface of zirconium hydride with n-propoxide zirconium as precursor. The effects of different heat treatment atmospheres on the cross-section morphology, surface morphology, phase composition and hydrogen-occluding properties of ZrO2 films prepared by sol-gel method were investigated when the heat treatment temperature was 600 ℃. The cross-sectional morphology, surface morphology, phase structure and thickness of the zirconia film were measured by scanning electron microscopy (SEM), confocal laser scanning microscopy (CLSM), X-ray diffraction (XRD) and eddy current thickness measurement. Hydrogen evidencing performance of the film was evaluated by vacuum dehydrogenation experiments. The results show that when oxygen is present in the heat treatment atmosphere, a continuous and dense zirconium oxide film can be obtained on the surface of zirconium hydride. When the heat treatment atmosphere is in the absence of oxygen, the prepared zirconium oxide film is discontinuous and uniform Poor sex. The hydrogen barrier effect of the zirconium oxide film prepared under aerobic atmosphere is better than that under anaerobic condition. The film thickness is 10.1μm, and the PRF value is 8.4. However, the microstructure of ZrO2 film was not affected by the different heat treatment atmosphere. The film mainly consisted of monoclinic zirconia M-ZrO2 and tetragonal zirconia TZrO2, and mainly consisted of monoclinic zirconia M-ZrO2.