To generate hydrogen from its storage as NaBH4, a catalyst was synthesized via an electrochemical method. The catalyst, Ni-Co, had hydroxyapatite as a support catalyst. The electrochemical cell consisted of a DC power supply, a carbon anode and cathode, and a bipolar membrane to separate the cell into two chambers. The current density was adjusted to 61, 91, and 132 mA/cm2. The electrolysis time was 30, 60, and 90 min. The particles produced were analyzed by XRD and SEM/EDX and tested in the hydrolysis of NaBH4 for hydrogen generation.