The present work was concentrated mainly on the reaction processes of boro/carbothermal reduction (BCTR) of ZrO 2 with B 4 C and carbon in vacuum, and characterization of morphology and sinterability of the obtained ZrB 2 powder. Combining the thermodynamic calculations, X-ray diffraction results, and the trend of furnace pressure with temperature during synthesis, a detailed explanation of the reaction processes of BCTR was developed. Most of the ZrB 2 particles obtained at 16501C presented a nearly spherical morphology, whereas those synthesized at 17501C showed a nearly columnar morphology with an increased size. Compared with the powder synthesized at 17501C as well as the commercially additive-free powder used in the reported work, the ZrB 2 powder synthesized at 16501C showed a better sinterability due to its smaller particle size and lower oxygen content.