Crystallization of mesoporous silica SBA-15 in a high pressure hydrothermal environment

Mesoporous silica SBA-15 (with ～6?nm pore size and ～6?nm wall thickness) was exposed to a hydrothermal environment at 2 and 5?GPa. The p,T quenched products were investigated by powder X-ray diffraction and transmission electron microscopy. Infrared spectroscopy and thermogravimetric analysis of a sample subjected to 5?GPa at room temperature suggests functionalization of both inner and outer pore surface by silanol. Partial transformation to nano-sized (20–50?nm) coesite crystals with nonfaceted morphology was observed during short equilibration times of 2?h at 125°C, which is significantly below the melting point of water (～250°C). Untransformed SBA-15 maintained intact pore structure. At 175°C and during 8?h, SBA-15 transformed completely into faceted coesite crystals with dimensions 100–300?nm, suggesting Ostwald ripening and thus significant mass transport in the solid water environment. At 2?GPa the melting point of water is near 70°C. Partial transformation to nano-sized α-quartz was observed at 65°C and during 2?h. Untransformed SBA-15 partially pore collapsed. The reduced pore stability of SBA-15 at 2?GPa is attributed to the presence of liquid water in the pores due to melting point depression of confined water.