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We investigated the pore properties of inorganic membranes used in the hydrogen separation industry. A microporous SiON membrane derived from a preceramic polysiloxazane was pyrolyzed for the analysis of the porosity characteristics. The involved reactions were studied using a combination of thermogravimetry and infrared spectroscopy of the solids. The SiON membrane showed a dense microporous structure and successfully formed a coating layer of pores on the intermediate membrane. The BET surface area and pore volume showed maximum values (653.4 m 2 /g and 0.35 cm 3 /g, respectively) at a pyrolysis temperature of 500°C.