Mine Eiichi, Hirose Mitsuaki, Nagao Daisuke, Kobayashi Yoshio, Konno Mikio
Department of Chemical Engineering, Graduate School of Engineering, Tohoku University, 6-6-07 Aoba, Aramaki-aza, Aoba-ku, Sendai 980-8579, Japan.
J Colloid Interface Sci. 2005 Nov 1;291(1):162-8. doi: 10.1016/j.jcis.2005.04.077. Epub 2005 Jun 9.
A synthetic method for preparing submicrometer-sized titania particles is proposed, which is based on hydrolysis of titanium alkoxide with the use of a cosolvent and an amine catalyst for alkoxide hydrolysis. The preparation was performed with different amines of ammonia, methylamine (MA), and dimethylamine (DMA) in different solvents of ethanol/acetonitrile, ethanol/methanol, ethanol/acetone, ethanol/acetonitrile, and ethanol/formamide for 0.1-0.3 M water and 0.03 M titanium tetraisopropoxide (TTIP) at temperatures of 10-50 degrees C. The use of the ethanol/acetonitrile solvent with MA was required for preparing monodispersed, spherical particles. The number average of the titania particle sizes and their coefficient of variation were varied from 143 to 551 nm and from 5.7 to 20.6%, respectively, with reaction temperature and concentrations of water and MA. Colloidal crystals of titania particles fabricated with a sedimentation method revealed reflection peaks attributed to Bragg's diffraction. Annealing at 100-1000 degrees C led to shrinkage and crystallization of titania particles followed by an increase in the refractive index of titania particles.
提出了一种制备亚微米级二氧化钛颗粒的合成方法，该方法基于使用助溶剂和用于醇盐水解的胺催化剂对钛醇盐进行水解。在乙醇/乙腈、乙醇/甲醇、乙醇/丙酮、乙醇/乙腈和乙醇/甲酰胺等不同溶剂中，使用氨、甲胺（MA）和二甲胺（DMA）等不同胺类，在0.1 - 0.3 M水和0.03 M四异丙醇钛（TTIP）的条件下，于10 - 50℃的温度下进行制备。制备单分散球形颗粒需要使用含有MA的乙醇/乙腈溶剂。随着反应温度、水和MA浓度的变化，二氧化钛颗粒的数均粒径及其变异系数分别在143至551 nm和5.7至20.6%之间变化。用沉降法制备的二氧化钛颗粒胶体晶体显示出归因于布拉格衍射的反射峰。在100 - 1000℃退火导致二氧化钛颗粒收缩和结晶，随后二氧化钛颗粒的折射率增加。
