Nickel ferrites composite catalysts with the spinel structure were synthesized by the coprecipitation method. Nickel ferrites were deposed on the surface of industrial active carbon. The temperature of final calcination in inert media was 400, 500, and 600°C. The trevorite phase was determined by XR-diffraction; the ratio of Ni to Fe was checked by luminescent analysis, it consisted ~0.61. Crystallites sizes varied in the range from 218 to 252 nm and decreased with an increase in the calcination temperature. It was found that the rate of hydrogen evolution in the reaction of sodium borohydride hydrolysis increases with the reaction temperature increasing; catalysts obtained at lower calcination temperatures showed higher catalytic activity. The maximum Hydrogen Generation Rate (2181 ml×min-1×g-1) was observed for nickel ferrite deposited on the active carbon and calcined at a temperature 400oC; the activation energy of the reaction in the presence of this composite ferrite consisted ~50 kJ×mol-1.