| TiO2-ZrO2聚合溶胶形成过程的小角X射线散射研究 |
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| 引用本文： | 杜倩倩,谷景华,默广,魏彦茹,殷文杰,李甲. TiO2-ZrO2聚合溶胶形成过程的小角X射线散射研究[J]. 化工学报, 2018, 69(4): 1731-1740. DOI: 10.11949/j.issn.0438-1157.20170730 |
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| 作者姓名： | 杜倩倩 谷景华 默广 魏彦茹 殷文杰 李甲 |
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| 作者单位： | 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 |
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| 基金项目： | 国家自然科学基金项目（51178017）。 |
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| 摘 要： | 由金属醇盐（M（OR）4）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。通过控制异丙醇钛[Ti（i-OC3H7）4]和正丙醇锆[Zr（n-OC3H7）4]的混合物在异丙醇（i-C3H7OH）中水解制备聚合型TiO2-ZrO2溶胶，利用小角X射线散射方法（SAXS）研究了初始反应混合物Ti（i-OC3H7）4：Zr（n-OC3H7）4：H2O：i-C3H7OH=0.9：0.1：m：30（摩尔比，m=1.8，2.0，2.2）形成TiO2-ZrO2溶胶的过程，探讨了水与醇盐摩尔比H2O/M（OR）4（M=Ti+Zr）、反应温度和正丙醇锆对TiO2-ZrO2溶胶形成的影响。研究结果表明，H2O/M（OR）4=1.8时，只有少量胶粒形成；H2O/M（OR）4=2.0～2.2时，TiO2-ZrO2溶胶中胶粒具有质量分形结构，分形维数1.2 ≤ Dm < 1.4；随着H2O/M（OR）4增加，胶粒的形成时间缩短，胶粒大小和分形维数均增大，溶胶的稳定性显著下降。升高反应温度有利于胶粒形成。[Ti（i-OC3H7）4+Zr（n-OC3H7）4]混合物比Ti（i-OC3H7）4水解快，H2O/M（OR）4相同时，TiO2-ZrO2溶胶比TiO2溶胶稳定性差。
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| 关 键 词： | 金属醇盐水解 SAXS 聚合溶胶 TiO2-ZrO2溶胶 胶粒分形 |
| 收稿时间： | 2017-06-05 |
| 修稿时间： | 2017-10-09 |
Study on formation of polymeric TiO2-ZrO2 sols by small angle X-ray scattering |
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| DU Qianqian,GU Jinghua,MO Guang,WEI Yanru,YIN Wenjie,LI Jia. Study on formation of polymeric TiO2-ZrO2 sols by small angle X-ray scattering[J]. Journal of Chemical Industry and Engineering(China), 2018, 69(4): 1731-1740. DOI: 10.11949/j.issn.0438-1157.20170730 |
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| Authors: | DU Qianqian GU Jinghua MO Guang WEI Yanru YIN Wenjie LI Jia |
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| Affiliation: | 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 |
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| Abstract: | Metal oxide sols can be prepared from metal alkoxides M(OR)4 by hydrolyzation, which has been widely used in synthesis of nano-porous ceramic membranes by sol-gel method. Polymeric TiO2-ZrO2 sols were prepared by controlled hydrolyzation of the mixture of titanium isopropoxide and zirconium n-propoxide in isopropanol. The formation of TiO2-ZrO2 sols from the initial reactant mixtures with a molar ratio of Ti(i-OC3H7)4:Zr(n-OC3H7)4:H2O:i-C3H7OH=0.9:0.1:m:30 (m=1.8, 2.0, 2.2) was investigated by small angle X-ray scattering (SAXS). The effects of the molar ratio of water to metal alkoxides H2O/M(OR)4 (M=Ti+Zr) in the initial reactant mixture, reaction temperature and Zr(n-OC3H7)4 on formation of TiO2-ZrO2 sols were discussed. When the molar ratio of H2O/M(OR)4=1.8, a few colloidal particles form. When the molar ratio of H2O/M(OR)4 is in the range of 2.0-2.2, the colloidal particles in TiO2-ZrO2 sols have a mass fractal structure with a fractal dimension of 1.2 ≤ Dm < 1.4. As the molar ratio of H2O/M(OR)4 increases from 2.0 to 2.2, the duration of colloidal particle formation becomes shorter, the size and fractal dimension of colloidal particles increase, and the stability of TiO2-ZrO2 sol decreases. Furthermore, the mixture of[Ti(i-OC3H7)4+Zr(n-OC3H7)4] hydrolyzes faster than Ti(i-OC3H7)4. TiO2-ZrO2 sol has lower stability than TiO2 sol from the initial reactant mixtures with the same molar ratio of H2O/M(OR)4. |
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| Keywords: | hydrolysis of metal alkoxides SAXS polymeric sol TiO2-ZrO2sol fractal dimension of colloidal particle |
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