Preparation of Spherical Hexagonal Mesoporous Silica

Abstract

A series of hexagonal mesoporous silica (HMS) have been synthesized by the neutral assemble pathway in water-alcohol cosolvent systems, using dodecylamine (DDA) and tetraethyl orthosilicate (TEOS) as the starting materials. These materials were characterized with powder X-ray diffraction, nitrogen sorption measurement, differential thermal analysis, and transmission electron microscopy. The XRD patterns of these samples exhibited a strong intense reflection at low angle, suggesting the excellent mesostructures of the samples. The particle size of HMS decreased and the morphology of HMS exhibited high textural porosity as the HMS was prepared with high addition rate of TEOS. The particle size of HMS prepared without aging was smaller than that aged for 18 h, due to the reaction time of TEOS was not enough to form complete particles. Addition of NaCl and HCl hindered the formation of HMS mesoporous structure. In contrast, addition of 1-butanol did not affect the formation of HMS mesoporous structure. The sphereical HMS silica with uniform size has been synthesized by adjusting DDA and TEOS concentrations. The shape of HMS became larger and more spherical as the concentrate on of DDA decreased. The stirring rate of the reaction mixture had no effect on either the shape or the size of the spheroid HMS silicas. However, the particles started to crack at higher stirring rates.