Microporous polystyrene membranes were prepared by the phase separation process using the supercritical CO2 as a nonsolvent for the polymer solution. The thin polymer solution in a laboratory dish was located inside a cell and the supercritical CO2 was introduced to induce the phase separation. The dry flat microporous membranes were obtained without collapse of the structure after the CO2 pressure was diminished. Effects of the experimental conditions such as the CO2 pressure, the polymer concentration and the temperature on the average pore size and membrane porosity were investigated.