Polymethyl methacrylate (PMMA) was prepared by solution polymerization method. Different concentrations (10, 20 and 40%) of Ni powder were dispersed in PMMA and the composite films were prepared by casting method. These films were irradiated with 120 MeV Ni10 + ions at a fluence of 5 × 1012 ions/cm2. Electrical, structural and chemical properties of the composites were studied by means of an LCR meter, X-ray diffraction, FTIR spectroscopy and SEM/AFM, respectively. The results showed that the conductivity increases with metal concentration and also with ion beam irradiation. This reveals that ion beam irradiation promotes the metal/polymer bonding and converts polymeric structure into hydrogen depleted carbon network. It was observed from XRD analysis that percentage crystallinity and crystalline size decrease upon irradiation. This might be attributed to rupture of some polymeric bonds, which is also corroborated with FTIR spectroscopic analysis. Ion beam tempts graphitization of polymeric material by emission of hydrogen and/or other volatile gases. Surface morphology of the pristine and irradiated films was studied by atomic force microscopy (AFM)/scanning electron microscopy (SEM). Result showed that the surface roughness increases after ion beam irradiation.