Metal oxycarbide solid solution possesses an extensive potential applications due to its remarkable physical features. In this paper, TaCxO1-x solid solution is successively and controllably synthesized by carbothermal reduction of Ta2O5. Based on the thermodynamic calculation, the possible reactions under different conditions in the carbothermal reduction process were analyzed, which provides theoretical guidance for controllable regulation and optimization of carbon thermal reduction process. The effects of carbon content, sintering temperature, and holding time on the synthesis of TaCxO1-x solid solution were investigated and the ideal process parameters for the synthesis of single-phase solid solution were identified. A single-phase solid solution with a carbon‑oxygen ratio close to 1:1 can be created as a soluble anode if the synthesis temperature is 1500 °C, the holding period is 6 h, and the molar ratio of C/Ta is 3.42. Moreover, the process feasibility of preparing metal tantalum by electrolysis of tantalum-based soluble anode is discussed, which provides a new method for metal tantalum preparation.