For the first time the synthesis of poly(N-vinyl-2-pyrrolidone)-stabilized cobalt-palladium nanoparticles by an easy method, their characterization, and their use as active catalysts for hydrogen release from hydrolysis of ammonia borane and hydrazine borane is reported here. The catalyst is prepared by simultaneous reduction of suitable cobalt and palladium ions by sodium borohydride in the presence of poly(N-vinyl-2-pyrrolidone) as a stabilizer. They are characterized by UV-Vis spectroscopy, TEM analysis, X-ray diffraction, and X-ray photoelectron spectroscopy. They provide average turnover frequencies of 30 min(-1) and 45 min(-1) in the hydrolysis of ammonia borane and hydrazine borane. They also provide activation energies of 48.6 +/- 2 and 50.6 +/- 2 kJ mol(-1) in the hydrolysis of ammonia borane and hydrazine borane.