Controlling the Pore Size and Morphology of Mesoporous Silica

Abstract: Mesoporous silica with a hexagonally ordered pore structure (SBA-15) has been synthesized. Through variations in the synthesis conditions several morphologies, such as fibers, sheets and separate rods, have been realized. Furthermore, additions of heptane and NH4F make it possible to synthesize SBA-15 with pores as large as 18 nm in the sheet morphology. Mechanisms for the formation of different morphologies have been suggested. In the case of fibers and sheets, the amount of heptane present during the synthesis determines the final morphology. For low concentrations, the heptane enters the micelles and increases the pore size while the particles (crystallites) attaches to each other end to end. When the heptane concentration increases, the heptane droplets increase in size, and above a critical droplet size the crystallites attach with one short end towards the droplet, forming the sheet morphology. The crystallites can also be separated. This is the case of the rod morphology. The separation is performed by shortening the stirring time and increasing the HCl concentration. The increased amount of HCl increases the hydration rate of the silica precursor, which can be used to control the thickness and length of the rods. Furthermore, the reaction time has been decreased from 20 h for all morphologies to less than 4 hours. The materials have been characterized with nitrogen sorption, electron microscopy and x-ray diffraction. Also, thermogravimetric analysis and fourier transformed infrared spectroscopy have been used for studying the removal of surfactants.