Pure and ZnO-doped Ni0.1Co0.9Fe2O4 catalyst were prepared by co-precipitation method and thermal decomposition in air calcinated at 400-700°C and that treated with different amounts of zinc nitrate (0.46-2.25 w% ZnO). X-ray powder diffractometry, scanning electron microscopy (SEM) and BET analysis of nitrogen adsorption isotherms investigated the crystalline bulk structure and the surface area of pure and doped samples, respectively. The hydrogen peroxide decomposition activity was determined by oxygen gasometry of the reaction kinetics at 20-40°C. The results revealed that the treatment of Ni0.1Co0.9Fe2O4 with ZnO at 400-700°C brought about a significant increase in the specific surface area and catalytic activity of Ni0.1Co0.9Fe2O4 on decomposition of hydrogen peroxide. However, the catalytic activity of H2O2 decomposition on Ni0.1Co0.9Fe2O4 calcined at different temperatures was found to show a considerable increase by doping with ZnO. They were discussed with UV/VIS spectroscopy which the energy band gap of the synthesized Ni0.1Co0.9Fe2O4 nano structure was calculated to be ~5 eV.