The optimization of a novel anode for the production of hydrogen via an ammonia alkaline electrolytic cell is presented. The novel anode is prepared by electrodeposition and contains Raney nickel, platinum and rhodium in its catalytic layer. Optimization of current density and charge density for deposition of the Raney nickel layer is performed via a factorial design experimental method to maximize the percentage of Raney nickel powder on a titanium grid. The platinum and rhodium layers are optimized by considering their influence on reaction kinetics. It is proven by electrochemical analysis that platinum and rhodium realize a synergistic catalytic effect on the oxidation of ammonia, showing higher activity than platinum-only electrodes with comparable catalyst loading. Hydrogen is successfully produced from a 1 M NH3 / 5 M KOH solution at 14.54 Wh/g H2 by an anode containing 1 mg/cm2 Rh and 10 mg/cm2 Pt at ambient temperature and pressure.