热处理温度对溶胶-凝胶法制备ZrH_(1.8)表面氧化锆膜层的影响

Characteristics of Zirconia Films Prepared by Sol-Gel Method on Surface of ZrH_(1.8) at Different Heat Treatment Temperatures

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。

For preventing hydrogen loss from zirconium hydride,zirconium oxide films were prepared on the surface of zirconium hydride by Sol-Gel method.Zirconium n-propoxide was as precursor in the reaction system.The influence of heat treatment temperature on phase composition,surface morphologies,cross-sectional morphologies and hydrogen resistance performance of zirconium oxide films were researched by X-ray diffractometer（XRD）,confocal laser scanning microscope（CLSM） and scanning election microscopy（SEM）,respectively.Hydrogen resistance performance was evaluated by the experiment of vacuum dehydrogenation testing.The results show that the continuous and dense zirconium oxide films form on the surface of zirconium hydride when heat treatment temperature is above 600 °C.The PRF（permeation reduction factor） values of zirconium oxide films increase at first,and then decrease with increasing of heat treatment temperature.The maximum PRF value of zirconium oxide films reaches 8.6 at 600 °C.The phase structure of zirconium oxide films is both tetragonal phase T-ZrO2 and monoclinic phase M-ZrO2,and the films are mainly composed of monoclinic phase M-ZrO2.