硅烷偶联剂对制备硅酸锆薄膜及其抗氧化性能的影响

采用乙酸锆和正硅酸乙酯为原料, 硅烷偶联剂3-氨丙基三乙氧基硅(APTES)为表面改性剂, 通过溶胶-凝胶法制备了致密硅酸锆薄膜。系统研究了APTES的添加对硅酸锆薄膜的晶体结构、显微形貌及其抗氧化性能的影响。实验结果表明, 添加硅酸锆摩尔浓度10mol%的APTES可以制备出纯相的致密硅酸锆薄膜, 超过这一浓度则会出现少量的SiO₂杂质, 同时造成硅酸锆溶胶的黏度迅速升高。AFM测试结果表明添加APTES制备的薄膜更致密平滑。1300℃抗氧化测试102 h后, 未镀膜的碳化硅基底增重0.16%, 相比之下, 添加APTES前后的样品的增重分别为0.08% 和0.03%, 说明添加APTES有利于提高ZrSiO₄薄膜的致密度, 进而提高其抗氧化性能。

Silane Coupling Agent on Synthesis and Antioxidation Property of Zircon Film

The dense zircon film was prepared via Sol-Gel method using zirconium acetate and tetraethoxysilane as raw materials, and silane coupling agent 3-aminopropyltriethoxysilane (APTES) as surface modifying agent, respectively. Influences of APTES on the phase composition, morphology and antioxidation property of the ZrSiO₄ film were investigated. The experiment results indicated that the pure and dense zircon film was achieved with addition of 10mol% APTES into ZrSiO₄ sol. Once the molar ratio of APTES was beyond 10mol%, the impurity SiO₂ was observed, and the viscosity of the ZrSiO₄ sol increased significantly at the same time. AFM results showed that the smooth and dense film was obtained with APTES addition. After 102 h oxidation cyclic test at 1300℃, uncoated SiC substrate gained weight of 0.16%, while samples coated with ZrSiO₄ thin films only gained weight of 0.08% and 0.03% before and after addition of APTES. In summary, APTES addition is beneficial for the density of ZrSiO₄ thin film, resulting in excellent anti-oxidation property.