Thermodynamic calculation and kinetic analysis were performed on the carbothermal reduction process of Co 3O 4–Sb 2O 3–C system to clarify the reaction mechanism and synthesize pure CoSb powder for the anode material of secondary lithium-ion batteries. The addition of carbon amount and thus the purity of CoSb powders were critical to the electrochemical property of CoSb anode. It was revealed that in an inert atmosphere, Co 3O 4 was preferentially reduced to CoO, followed by the reduction of Sb 2O 3 and CoO. CO 2 was the gas product for the reduction of Co 3O 4 and Sb 2O 3, while CO was the gas product for that of CoO. Based on the analysis result, pure CoSb powder without any oxides and residual carbon was synthesized, which showed a higher specific capacity and a lower initial irreversible capacity loss, compared to CoSb sample with residual carbon. This work can be a reference for other carbothermal reduction systems.