In this study, a new nanocatalyst, RuBi/carbon nanotube, was synthesized to be used in the hydrolysis reaction of sodium boron hydride. The sodium boron hydride hydrolysis performance was investigated by adding bismuth to the structure of ruthenium nanocatalysts. Hydrolysis experiments were carried out by adding bismuth at different atomic proportions to ruthenium. The best atomic ratio was determined to be 90:10. These catalysts are characterized by scanning electron microscopy with energy-dispersive X-ray analysis, X-ray diffraction, and transmission electron microscopy. The parameters affecting hydrolysis such as temperature, catalyst amount, sodium hydroxide concentration, and sodium borohydride concentration were examined. The reusability of the catalyst was tested five times. In the calculations, the reaction order was calculated as n, 0.73, and activation energy E-a, 49657 kJ/mol.