采用溶胶凝胶法在氢化锆表面制备防氢渗透膜层,分析了不同前驱体溶胶浓度对氢化锆表面膜层的性能影响。借助XRD、SEM等分析手段对氧化层的物相组成和形貌进行分析,并采用真空脱氢试验测试氧化层的阻氢性能PRF值(permeation reduction factor)。试验表明,在前驱体溶胶浓度范围内可制膜层厚度为5~14.3μm,膜层厚度随着溶胶浓度升高呈现先升高后下降的趋势。当溶胶浓度低于1.0 mol/L时,不易生成连续完整的膜;当溶胶浓度高于1.0 mol/L时,膜层表面出现了颗粒堆积和裂纹,膜层不连续。氧化物的相结构无明显改变,以单斜相M-Zr O2和四方相T-Zr Ox为主;氧化层的PRF值在9.86~10.43之间变化。
Zirconia coatings as hydrogen were formed on disk-type Zr H2 substrate by a sol-gel method. Properties of oxide coatings were studied with different precursor concentrations. The phase structure and morphology of oxide coatings were analyzed by XRD and SEM,respectively. The anti-permeation effect was tested by a vacuum dehydrogenation experiment. Results show that the thickness of total oxide coatings varied from 5 μm to 14.3 μm, which increased first and then decreased with the precursor concentration increasing. SEM images of oxide coating morphology and cross section demonstrate the continuous coatings couldn't be generated when the concentration was set below 1.0 mol/L; however, when the concentration was higher than 1.0 mol/L, particle accumulation and cracks occurred on the surface of the coating and the coating was not continuous. The phase structure of the oxide coating is monoclinic Zr O2 and tetragonal Zr Ox.Permeation reduction factor values range from 9.86 to 10.43.