Abstract In this research the effect of mechanical alloying on the in situ synthesis–sintering behavior and mechanical properties of MoSi2 has been investigated. The Mo and Si powders according to MoSi2 stoichiometric composition were mechanically alloyed at different times. Then, the powders were subjected to spark plasma sintering process for preparing monolithic MoSi2. X-ray diffraction pattern of the sintered samples showed that by increasing the mechanical alloying time, Mo5Si3 has been formed. It seems that the formation of Mo5Si3 is due to the effect of mechanical alloying on microstructure and thermodynamic condition of the reaction.