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人工晶体学报 ›› 2017, Vol. 46 ›› Issue (12): 2393-2398.

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非水解溶胶-凝胶法制备硅酸锆薄膜及抗碱腐蚀性能

谭广繁;胡庆;江伟辉;刘健敏;冯果;陈婷;李聪   

  1. 景德镇陶瓷大学材料科学与工程学院,景德镇,333403;景德镇陶瓷大学材料科学与工程学院,景德镇333403;国家日用及建筑陶瓷工程中心,景德镇 333001;国家日用及建筑陶瓷工程中心,景德镇,333001
  • 出版日期:2017-12-15 发布日期:2021-01-20
  • 基金资助:
    国家自然科学基金(51362014,51602136);江西省自然科学基金(20171BAB216010);江西省教育厅基金(GJJ160918)

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

TAN Guang-fan;HU Qing;JIANG Wei-hui;LIU Jian-min;FENG Guo;CHEN Ting;LI Cong   

  • Online:2017-12-15 Published:2021-01-20

摘要: 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(ZrSiO4)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ZrSiO4合成、ZrSiO4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1 mm/s时可以在单晶硅片获得表面光滑、平整致密、无开裂的ZrSiO4薄膜.镀有ZrSiO4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ZrSiO4薄膜具有较好的抗碱液腐蚀性能.

关键词: 硅酸锆;薄膜;非水解溶胶-凝胶法;抗腐蚀

Abstract: 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 ZrSiO 4 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 ZrSiO 4 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 ZrSiO 4 film was soaked in 40; NaOH solution for 42 h at 40 ℃, 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 ZrSiO 4 film had good alkali corrosion resistance .

Key words: 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 ZrSiO 4 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 ZrSiO 4 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 ZrSiO 4 film was soaked in 40; NaOH solution for 42 h at 40 ℃, 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 ZrSiO 4 film had good alkali corrosion resistance .

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