非水解溶胶-凝胶法制备硅酸锆薄膜及抗碱腐蚀性能

Preparation of Zirconium Silicate Film by Non-Hydrolytic Sol-Gel Method and Its Alkali Corrosion Resistance

以正丙醇锆和正硅酸乙酯分别为锆源和硅源,结合非水解溶胶-凝胶法和提拉镀膜工艺制备出硅酸锆(ZrSiO_4)薄膜。采用XRD、FTIR、SEM、AFM等分析测试手段研究了前驱体浓度、提拉速度对ZrSiO_4合成、ZrSiO_4薄膜形貌及显微结构的影响,并研究薄膜的抗碱液腐蚀性能。结果表明:当前驱体浓度为0.1 mol/L、提拉速度为1mm/s时可以在单晶硅片获得表面光滑、平整致密、无开裂的ZrSiO_4薄膜。镀有ZrSiO_4薄膜的单晶硅片在浓度为40%NaOH溶液中40℃条件下浸泡42 h,表面只发现有较小的坑蚀,且质量随腐蚀时间延长变化很小,质量损失仅为0.17%,表明该ZrSiO_4薄膜具有较好的抗碱液腐蚀性能。

Zirconium silicate （ZrSiO4 ） film was prepared via non-hydrolytic sol-gel method （NHSG） combining dip coating process using Zirconium propoxide as zirconium source and tetraethyl orthosilicate as silicon source. The effects of precursor concentration and lifting rate on the morphology, microstructure and alkali corrosion resistance of ZrSiO4 film were investigated by X-ray diffraction （XRD） , Fourier transform infrared spectrometer （FTIR）, Scanning electron microscopy （SEM） and Atomic force microscope （AFM）, respectively. The results show that the smooth and dense ZrSi04 film without cracking could be coated on the monocrystalline silicon when the precursor concentration is 0.1 mol/L and the lifting rate is 1 mm/s. Monocrystalline silicon coated ZrSi04 film was soaked in 40% NaOH solution for 42 h at 40 ~C, only a relatively small pit corrosion on the surface was found, the mass varies a little with the corrosion time and the mass loss was only 0.17% , which indicate that the ZrSiO4 film had good alkali corrosion resistance.