Preparation of particulate/polymeric sol–gel derived microporous silica membranes and determination of their gas permeation properties

Monodisperse silica sols with well-defined spherical particles ranging in size from 5 to 310 nm were prepared through Stober process. Both particulate and polymeric sol–gel routes were employed for the preparation of stable silica sols. The use of polymeric species in combination with particulate silica spheres may allow the design of predefined membrane pore structures with high thermal stability by cubic/random/close packing of monodisperse spherical particles incorporated into the polymeric network. The size and volume content of spheres were varied in order to modify the consolidation behaviour of 2-structural silica membranes which would enhance the thermal stability. The low shrinkage level for sphere loaded 2-structural systems compared to the pure polymeric counterparts might be explained by the decrease in the structural free energy of the polymeric/particulate 2-structural system. The thermal stability of the microporous membranes may thus be improved by incorporating particulates into the polymeric network through the formation of a lower extent of thermally induced microcrack formation. The N2 permeation through 90 nm silica sphere added silica membranes remained constant when they were heat treated in the 250–400 °C range indicating the stability of the pore network.