Supported catalysts are of great interest because of their wide range of application possibilities. In this study, firstly silica spheres were synthesized and then platinum and nickel nanoparticles were incorporated on this silica by microwave irradiation, which is an efficient technique for catalyst preparation. Synthesized silica spheres and catalysts were characterized by BET, X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetric analysis, and transmission electron microscopy techniques. Pt or Ni nanoparticles well dispersed over silica support were obtained using microwave irradiation.