Novel mixed-matrix membranes based on polysulfone (PS) and fullerene C60 (up to 5 wt%) have been developed. Two membrane types formed from PS and PS-C60, a dense (diffusive) membrane and a supported membrane, consisted of a thin PS or PS-C60 selective layer (&5 lm) on the surface of hydrophobic fluorocarbon polymer porous support (MFFC) were studied. The effect of fullerene incorporation on the structure and physical and chemical properties of PS membranes were investigated by scanning electron microscopy, nuclear magnetic resonance, contact angle measurements, sorption experiments, and wideangle X-ray diffraction. The transport properties of the mixed matrix membranes containing up to 0.5 wt% fullerene were studied for the pervaporation of ethyl acetate–water mixture. The new mixed-matrix membranes, developed in this study, were selective to water, whereas the PS-0.5 % C60/MFFC composite membrane was found to have the best performance.