A marked improvement in gas separation properties of asymmetric membranes based on poly(vinyl trimethylsilane) containing traces of solvent and non-solvent used in membrane preparation was achieved by thermal treatment in a confined volume. Thermal treatment in a temperature range from 40 to 180 degrees C appeared to be effective, and exposure time was varied from one minute to several hours. Thermal treatment of the asymmetric membranes was shown to improve their stability after plasmochemical modification.