The synthesis of highly active and selective catalysts is the central issue in the development of hydrous hydrazine(N_2H_4·H_2O) as a viable hydrogen carrier. Herein, we report the synthesis of bimetallic Ni-Ir nanocatalyts supported on CeO_2 using a one-pot coprecipitation method. A combination of XRD, HRTEM and XPS analyses indicate that the Ni-Ir/CeO_2 catalyst is composed of tiny Ni-Ir alloy nanoparticles with an average size of around 4 nm and crystalline CeO_2 matrix. The Ni-Ir/CeO_2 catalyst exhibits high catalytic activity and excellent selectivity towards hydrogen generation from N_2H_4·H_2O at mild temperatures. Furthermore, in contrast to previously reported Ni-Pt catalysts, the Ni-Ir/CeO_2 catalyst shows an alleviated requirement on alkali promoter to achieve its optimal catalytic performance. The synthesis of highly active and selective catalysts is the central issue in the development of hydrous hydrazine (N 2 H 4 · H 2 O) as a viable hydrogen carrier. Herein, we report the synthesis of bimetallic Ni-Ir nanocatalyts supported on CeO 2 using a one-pot coprecipitation method. A combination of XRD, HRTEM and XPS analyzes indicate that the Ni-Ir / CeO 2 catalyst is composed of tiny Ni-Ir alloy nanoparticles with an average size of around 4 nm and crystalline CeO 2 matrix. In contrast to previously reported Ni-Pt catalysts, the Ni-Ir / CeO 2 catalyst shows an alleviated requirement on alkali promoter to achieve its optimal catalytic performance.