以氧氯化锆和正硅酸乙酯为锆源和硅源,采用溶胶-凝胶法制备硅酸锆薄膜.借助SEM、DTA-TG、FT-IR、XRD等分析测试手段研究了添加双氧水(H2O2)对制备硅酸锆薄膜的影响,并研究了薄膜的抗腐蚀性能.结果表明:适量的双氧水可以有效地促进氧氯化锆的水解,进而克服薄膜高温失重造成孔洞和致密性差的问题;当H2O2/Zr的摩尔比小于2时,制备的薄膜不致密、不均匀;当H2O2/Zr的摩尔比大于2时,制备的样品有杂质相;最优的H2O2/Zr摩尔比为2,可制得均匀、致密的硅酸锆薄膜;所制备的薄膜具有较好的抗NaOH溶液腐蚀性能,单晶硅基片腐蚀前后质量损失为16.92％,而镀有硅酸锆薄膜的单晶硅基片腐蚀前后质量损失仅为0.56％.
Zirconium silicate thin film was prepared via sol-gel method using zirconium oxychloide as zirconium source and tetraethyl orthosilicate as silicon source.The effects of hydrogen peroxide (H2O2)on the preparation of zirconium silicate film and the corrosion resistance of zirconium silicate film were investigated by means of SEM,DTA-TG,FT-IR and XRD,respectively.The results show that appropriate hydrogen peroxide effectively accelerates the hydrolysis of the zirconium oxychloide and overcomes the holes and poor densification caused by weight loss at high temperature.When the mole ratio of H2O2/Zr is less than 2,uniform and dense film can not be prepared.However,impurity phase appears when the mole ratio of H2O2/Zr is more than 2.Uniform and dense zirconium silicate thin film could be prepared when the optimal mole ratio of H2O2/Zr is 2.The thin film has excellent corrosion resistance against NaOH solution.The mass loss of silicon wafer is 16.92％ after corrosion,however,the mass loss of silicon wafer with zirconium silicate thin film is only 0.56％.
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