Abstract: Ammonia borane (NH₃BH₃, AB) is considered as an ideal hydrogen storage material for portable hydrogen production. In this paper, a bimetallic carbon cube (Co_0.8Cu_0.2/CNC) catalyst was prepared by high-temperature calcination of the Co_0.8Cu_0.2-ZIF precursor, which was obtained by stirring the reactants at room temperature. In addition, the microstruc-ture and composition of the catalyst were investigated using various characterization methods. The change regularity of the catalyst was explored through the single-variable method. The results showed that the addition of a small amount of Cu had a stabilizing effect on the cubic morphology of the Co_0.8Cu_0.2/CNC catalyst. When the dispersant was CTAB and the calcination temperature was 873 K, the activation energy (E_a) for catalyzing the hydrolysis of AB to hydrogen was 50.79 kJ/mol with the transition frequency (TOF) value as high as 23.37 min⁻¹. Moreover, the cata-lyst could still catalyze the complete hydrolysis of AB to hydrogen after 25 cycles, which indicated that the catalyst had good stability performance.