i 2 has potential application as a structural material. Synthesis of i 2 via mechanical alloying and combustion synthesis method was investigated. Nb and Si powders (Nb:Si=1:2) were alloyed by milling at different times. The products were identified by XRD analysis. No reaction takes place between Nb and Si at alloying times less than 10 hours. However the intensity of Si peaks decrease mainly due to dissolution of Si in Nb. i 2 formation is initiated at milling times higher than 20 hours, and nearly complete conversion to i 2 takes place after 60 hours. Combustion synthesis experiments were performed on reactant powder in thermal explosion mode at 1300 o C. The results showed that no reaction takes place in the reactant sample of Nb:Si=1:2 without mechanical alloying. At alloying times more than 10 hours, i 2 wahyhy; produced during combustion synthesis. Experimental evidences showed that increasing milling time, not only increases the intensity of i 2 peaks, but also decreases T c and T ig . After 60 hours of milling, T ig was found to be 921 o C.