Abstract: The effects of reduction temperature, C:Ga₂O₃ and holding time on the experimental results in the process of vacuum carbothermal reduction of Ga₂O₃ were studied. The results show that under the optimal experimental conditions of reduction temperature of 1323 K, C:Ga₂O₃ (molar ratio) of 4, and holding time of 150 min, the condensate is enriched in uniform granular form on the condensation cover. The reduction rate of Ga₂O₃ is 68.19%, and the condensation yield of the reduction product is 59.37%. The condensate phase is gold gallium and a small amount of Ga₂O₃ formed by disproportionation reaction. The metal gallium is fully enriched in the condensation process and is well separated from Ga₂O₃.