Abstract: To develop the preparation method of ZrC/Mo−Si metal silicide composites with the simple process, low energy consuming, and low cost, the ZrC/Mo−Si metal silicide composite nano-powders were prepared by one-pot electrolytic process in molten salt, using ZrSiO₄, MoO₃, and C as raw materials in this paper. The effects of solid cathode preparation process, carbon content (mass fraction), and carbon source type on the electrochemical synthesis of ZrC/Mo−Si metal silicide composite nano-powders were investigated. The results show that, the ZrC/Mo−Si metal silicide composite nano-powders are prepared by electrochemical reduction at 800 ℃ under 3.1 V for 15 h in CaCl₂‒NaCl eutectic molten salt, which are composed of nearly spherical particles with the particle size less than 50 nm. It is found that the carbon powders with the amorphous structure and relatively smaller particle size are more suitable as the carbon source for the electrochemical synthesis of ZrC/Mo−Si metal silicide composites. Moreover, the ratio of ZrC and metal silicide phases, as well as the composition of metal silicide in the final products, can be controlled by adjusting the carbon content in the original materials.