In this research, we investigated the effects of reduction atmospheres on the creation of the Mo-Si-B intermetallic compounds (IMC) during the heat treatments. For outstanding anti-oxidation and elevated mechanical strength at the ultrahigh temperature, we fabricated the uniformly dispersed IMC powders such as Mo5SiB2 (T2) and Mo3Si (A15) phases using the two steps of chemical reactions. Especially, in the second procedure, we studied the influence of the atmospheres (e.g. vacuum, argon, and hydrogen) on the synthesis of IMCs during the reduction. Furthermore, the newly produced IMCs were observed by SEM, XRD, and EDS to identify the phase of the compounds. We also calculated an amount of IMCs in the reduced powders depending on the atmosphere using the Reitveld refinement method. Consequently, it is found that hydrogen atmosphere was suitable for fabrication of IMC without other IMC phases.