Au and/or Ni nanoparticles were synthesized by radiolysis on TiO 2 (commercial P25) at various composition (metal content). The modified photocatalysts were characterized by High Resolution Transmission Microscopy (HRTEM), Energy-Dispersive X-ray Spectroscopy (EDS), UV-Vis Diffuse Reflectance Spectroscopy (DRS) and X-Ray Photoelectron Spectroscopy (XPS). The charge-carrier mobility was studied by Time Resolved Microwave Conductivity (TRMC). The photocatalytic activities were tested under UV-visible irradiation using polychromatic and monochromatic light (action spectrum analysis of apparent quantum efficiency). Surface modified TiO 2 with Au and Ni nanoparticles showed high photocatalytic activity for hydrogen evolution from aqueous methanol solution. The enhanced hydrogen evolution rate was obtained for TiO 2 co-modified with Au and Ni, where synergetic effect of the two metals was revealed. A very small amount of gold associated to nickel (atomic ratio Ni:Au 5:1 with a total optimized metal loading of 0.5at%) can induce a significant increase in H 2 formation.