YThe bifunctional efficient electrocatalysts for both hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) are in urgent need for the advanced overall water splitting (OWS) device. Restricted by the thermodynamic limitations of the catalytic active center for OER and the reaction kinetics limitations induced by the structure of the electrocatalysts, the development of OWS catalysts requires more effort. Herein, a porous carbon-based bimetal electrocatalyst of Mo0.84Ni0.16-Mo2C@NC nanosphere is prepared by hydrothermal treatment of PMo12@PVP@Zn/Ni-ZIF which is synthesized via one-pot self-assembled hydrothermal method. Our study confirms that the Mo-Ni alloy and Mo2C nanoparticles homogeneously distribute in nitrogen-rich carbon-based materials. Furthermore, the porous structure exposes rich active sites and increases the effective specific area for redox reactions. The obtained Mo0.84Ni0.16-Mo2C@NC catalyst requires low overpotentials of 151 and 285 mV to reach a current density of 10 mA cm(-2) towards the water reduction and oxidation in 1 M KOH solution, respectively, and possesses good catalytic stability for one day. This work introduces an advanced method for the synthesis of the bimetal electrocatalyst. (C) 2021 Published by Elsevier Inc.