Preparation of semi-activated carbon fibers (SACFs) using a precursor consisting of coal tar pitch and phenolic resin coated on glass fiber was investigated. Stabilization of the fiber structure by crosslinking both the phenolic resin and coal tar pitch was essential to achieving high surface areas during high temperature activation. The phenolic resin was cured by using aqueous catalyst (hydrochloric acid/formaldehyde) followed by oxidative stabilization of the pitch. A surface area of 1,206 m(2)/g based on the precursor was obtained through activation using carbon dioxide/steam at 880 degrees C. The pore size distribution was shown to be vary narrow using the Horvath-Kawazoe (HK) method.