CIESC Journal ›› 2017, Vol. 68 ›› Issue (9): 3607-3615.DOI: 10.11949/j.issn.0438-1157.20170263

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Study on controlled hydrolysis of titanium isopropoxide by small angle X-ray scattering

DU Qianqian1, GU Jinghua1, MO Guang2, WEI Yanru2, YIN Wenjie1, LI Jia1   

  1. 1 School of Materials Science and Engineering, Beihang University, Beijing 100191, China;
    2 Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100039, China
  • Received:2017-03-19 Revised:2017-05-19 Online:2017-09-05 Published:2017-09-05
  • Contact: 10.11949/j.issn.0438-1157.20170263
  • Supported by:

    supported by the National Natural Science Foundation of China (51178017).

异丙醇钛控制水解的小角X射线散射研究

杜倩倩1, 谷景华1, 默广2, 魏彦茹2, 殷文杰1, 李甲1   

  1. 1 北京航空航天大学材料科学与工程学院, 北京 100191;
    2 中国科学院高能物理研究所, 北京 100039
  • 通讯作者: 谷景华
  • 基金资助:

    国家自然科学基金项目(51178017)。

Abstract:

Metal oxide sols can be prepared from metal alkoxides by hydrolyzation, which has been widely used in synthesis of nano-porous ceramic membranes by sol-gel method. However, the knowledge on hydrolysis mechanism of metal alkoxides is very limited. In this paper, TiO2 sols were prepared by controlled hydrolyzation of titanium isopropoxide[Ti(i-OC3H7)4] in isopropanol (i-C3H7OH). The formation of TiO2 sols from the initial reactant mixtures with different molar ratios of H2O/Ti(i-OC3H7)4[Ti(i-OC3H7)4:H2O:i-C3H7OH=1:m:30] was charterized by small angle X-ray scattering (SAXS). The mechanism of formation and growth of colloidal particles is discussed. TiO2 sol with a particle size less than 10 nm can be obtained. The formation and growth of colloidal particles are remarkably influenced by the molar ratio of H2O/Ti(i-OC3H7)4. When the molar ratio of H2O/Ti(i-OC3H7)4 ≥ 2.0, the stability of TiO2 sol decreases with the molar ratio of H2O/Ti(i-OC3H7)4 increasing.

Key words: hydrolysis of titanium isopropoxide, SAXS, TiO2 sol, particle size distribution, stability, shape of colloidal particle

摘要:

由金属醇盐水解制备溶胶的方法已广泛应用于溶胶-凝胶法制备纳米孔无机膜,但对金属醇盐水解机理的认识十分有限。通过控制异丙醇钛[Ti(i-OC3H74]在异丙醇(i-C3H7OH)中水解制备TiO2溶胶,利用小角X射线散射(SAXS)方法研究了由不同H2O/Ti(i-OC3H74的反应混合物[Ti(i-OC3H74:H2O:i-C3H7OH=1:m:30(摩尔比)]形成TiO2溶胶的过程,探讨了控制Ti(i-OC3H74水解的过程中胶粒形成与长大的规律。研究结果表明,所合成的TiO2溶胶的胶粒粒径小于10 nm,胶粒的形成和长大与H2O/Ti(i-OC3H74摩尔比密切相关。H2O/Ti(i-OC3H74(摩尔比) ≥ 2.0时,随着H2O/Ti(i-OC3H74增加,溶胶的稳定性下降。

关键词: 异丙醇钛水解, SAXS, TiO2溶胶, 粒度分布, 稳定性, 胶粒形状

CLC Number: