Abstract The present work describes the synthesis and characterization of a series of hybrid organo-inorganic ion exchange membranes for its use in fuel cells. Membranes were cast from dispersions of inorganic fillers in sulfonated polystyrene-block- poly(ethylene-ran-butylene)-block-polystyrene solutions and Nafion solutions. Silica gel, SBA-15 and sepiolite, all of them functionalized with phenylsulfonic acid groups, were used as fillers. Sepiolite and silica gel were functionalized by grafting of the phenyl ring to the solid. SBA-15 was prepared by sol-gel reaction. Functionalization was done by two methods. First one consisted in incorporation of phenyl at the synthesis wile the second one consisted on grafting of the phenyl ring to the prepared solid. Fillers were sulfonated under an SO3 atmosphere. SEBS was sulfonated using acetyl sulphate as sulfonation agent. After sulfonation, SEBS was dissolved in a THF/Ethanol mixture. To prepare Nafion membranes, a commercial 5% in low molecular weight alcohols solution was employed. Fillers were characterized first by ionic exchange capacity and elementary analysis. By this way, appropriate fillers were chosen. Adsorption analysis and thermogravimetric analysis were done to the selected fillers. Particle size was obtained using SEM. Membranes were characterized by water uptake, ion exchange capacity, SEM, TGA, DSC, DMA, FTIR and proton conductivity measurement using impedance spectroscopy. From microstructural analysis was determined that sepiolite gives better reinforcement properties to the polymeric matrix. This behaviour is due to its lower particle size that allows better filler-matrix interaction. The conductivity measurements showed that fillers incorporation doesn’t affect the conductivity compared to the pristine polymer. This is due to fillers sulfonation. Sulfonated SEBS has better conductivity than Nafion. In the last chapter, single cell test of the membranes is described. Run test were performed under O2/H2 atmosphere varying temperature and pressure.