高等学校化学学报

高等学校化学学报

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甲基三乙氧基硅烷修饰的Ti3+/SiO2复合薄膜的发光性能

蓝芳1, 曹聪蕊1, 肖波1, 蒋晓东2, 袁晓东2, 江波1   

    1. 四川大学化学学院, 成都 610064;
    2. 中国工程物理研究院激光聚变研究中心, 绵阳 621900
  • 收稿日期:2008-05-08 修回日期:1900-01-01 出版日期:2008-10-10 发布日期:2008-10-10
  • 通讯作者: 江波

Luminescence Properties of Ti3+ Doped Methyltriethoxysilane Modified SiO2 Composite Coating

LAN Fang1, CAO Cong-Rui1, XIAO Bo1, JIANG Xiao-Dong2, YUAN Xiao-Dong2, JIANG Bo1*   

    1. College of Chemistry, Sichuan University, Chengdu 610064, China;
    2. Research Center of Laser Fusion, China Academy of Engineering Physical, Mianyang 621900, China
  • Received:2008-05-08 Revised:1900-01-01 Online:2008-10-10 Published:2008-10-10
  • Contact: JIANG Bo

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摘要： 采用溶胶-凝胶(Sol-Gel)法, 以正硅酸乙酯(TEOS)和甲基三乙氧基硅烷(MTES)为先驱物, 盐酸为催化剂, 用二步水解法制备了Ti3+/SiO2薄膜和甲基三乙氧基硅烷修饰的Ti3+/SiO2复合薄膜. 采用红外光谱仪、X射线衍射仪、椭偏仪、荧光光谱仪等对膜层性质进行了分析. 结果表明, 掺杂Ti3+的SiO2薄膜分别在250 nm附近有一弱的激发峰, 294 nm附近有一强的激发峰, 在393 nm附近出现一强的发射峰. IR光谱发现, MTES修饰的Ti3+/SiO2复合薄膜的Si—OH的吸收峰强度比Ti3+/SiO2薄膜的略减小, Si—O—Si的吸收峰明显增强, 表明复合薄膜硅氧网络结构更规则, 有利于Ti3+的均匀分散. Ti3+/SiO2薄膜与复合薄膜的孔隙率分别为13.64%和6.66%, 表明MTES的加入使薄膜更致密. 在空气中陈放30 d后, Ti3+/SiO2薄膜已经检测不到荧光发射峰, 而MTES修饰的Ti3+/SiO2复合薄膜荧光强度只下降了18%. 在氮气中陈放30 d后, 普通薄膜与复合薄膜的荧光强度均仅下降了10%. 表明Ti3+的荧光猝灭的主要原因是由于Ti3+被氧化造成的. 溶胶中加入MTES后, 薄膜表面结构得到改善, 有效地防止了Ti3+的氧化, 荧光强度更稳定.

关键词: 三氯化钛, 甲基三乙氧基硅烷, 二氧化硅薄膜, 溶胶-凝胶, 发光性能

Abstract: Titanium trichloride doped silica coating modified by methyltriethoxysilane(MTES) was prepared by sol-gel method using two steps hydrolytic condensation with tetraethoxysilane(TEOS) and MTES as the precursors and hydrochloric acid as the catalyst. The properties of the coating were characterized with IR spectroscopy, X-ray diffractometer, spectroscopic ellipsometry and luminescence spectroscopy. The result showed that Ti3+ doped SiO2 coatings gave an excitation spectrum with two maxima, one at the wavelength of 250 nm, the other at the wavelength of 294 nm. Strong emission of Ti3+ doped SiO2 coatings was observed with a maximum at 393 nm. The Si—OH peak of MTES modified SiO2 composite coating is appreciably weaker and the Si—O—Si absoption peak is stronger than the normal Ti3+/SiO2 coating, which indicates that the silicon-oxygen network is improved by addition of MTES. Calculation results show that the porous ratio of the MTES modified Ti3+/SiO2 composite coating was reduced from 13.64% to 6.66%, indicating that the composite coating is much more compact. When the samples were aged in air at 25 ℃ for 30 d, the fluorescence disappeared completely for normal Ti3+/SiO2 coating, while the fluorescence intensity of the MTES modified Ti3+/SiO2 composite coating was only reduced by 18%. When aged in N2 atmosphere at 25 ℃ for 30 d, the fluorescence intensities of both coatings were reduced by only 10%, Showing that the primary reason of fluorescence quenching is oxidization of Ti3+. Addition of MTES in the sol can effectively improve the surface structure of SiO2 coating, which prevents Ti3+ from oxidization leading to a coating with stable fluorescence properties.

Key words: Titanium trichloride, Methyltriethoxysilane, Silica coating, Sol-gel, Luminescence property

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