Polymer Electrolyte Fuel Cells (PEFCs) offer low weight and high power density and are being considered for automotive and stationary power production besides space and electronic applications. In this work, gamma radiation effects on carbon materials (carbon powder and multi walled carbon nanotubes) used as substrates in PEFCs electrodes, were studied. The enhancing of free radicals formation (especially on carbon powder) was observed and studied by EPR spectroscopy. This evidence leads to a significant activation of carbon materials because paramagnetic sites represent the preferential position for platinum electrocatalyst nucleation. Galvanostatic techniques were applied to deposits platinum nanoparticles on carbon substrates while FEG-SEM characterization and cyclic voltammetry (CV) were carried out to study the morphology and the electrochemical performances of PEFCs electrodes.