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Silica microspheres are of much interest in several areas, such as liquid chromatography, medicine, biochemistry, colloidal chemistry and aerosol research. In this study, the sol−gel method was used to prepare these microparticles followed by three different drying processes. The first process involved intermittent supercritical fluid drying (SCF-I) using intermittent supercritical carbon dioxide (scCO 2 ) at a low temperature. The second approach involved continuous supercritical fluid drying (SCF-C) using continuous scCO 2 at low temperature, as well. The third approach involved vacuum drying (WO), which is a high temperature process. All of the experiments led to the successful precipitation of silica microparticles in the micrometre range. In all of the cases, a spherical morphology and no agglomeration were observed. The optimum preparation conditions were determined as follows: stirring speed is 200 r/min; continuous phase/dispersed phase is 2/1; Span® 80/ Tween® 20 is 5/2; the ratio of surfactant is 17%. In addition, the primary textural characteristics of these microspheres were investigated by nitrogen physisorption experiments. The results indicated that the size of the pore volume is as follows: V SCF-C > V SCF-I > V WO . The BET data indicate that the specific surface area of the porous silica microspheres is as follows: S SCF-C > S SCF-I > S WO .