Abstract: Using a proprietary molybdenum trioxide vapor-phase reduction apparatus, we successfully carried out the sublimation and reduction of MoO3. We investigated the effects of temperature on the sublimation rate of molybdenum trioxide and the particle size of the powder obtained through reduction. Through optimization of the sublimation and reduction processes, we produced pure molybdenum powder with fine and uniform particle size. The pure molybdenum powder was then subjected to capacitive discharge sintering. By investigating the effects of voltage and pressure on the microstructure and properties of metallic molybdenum, rapid densification of the molybdenum metal was ultimately achieved. The results indicate that as the sublimation temperature increases, the sublimation rate gradually increases, but the particle size of the sublimation products also gradually increases. Furthermore, when the temperature exceeds 900 ℃, the particle size distribution of the sublimation products widens significantly. Therefore, the optimal sublimation temperature that balances sublimation efficiency and product particle size uniformity is 850 °C. When the reduction temperature exceeds 1100 °C, the particle size of the molybdenum powder gradually increases with rising temperature. Reduction at 1100 °C yields near-spherical molybdenum powder with small particle size and uniform distribution. Furthermore, using capacitive discharge sintering under conditions of 30 V voltage and 60 MPa pressure, the density of the molybdenum billet can be instantly increased to 94.56%.