Mechanical alloying and pulse discharge sintering (MA-PDS) process was employed to fabricate MoSi
2 alloys with additions of Al, B or Nb alloy elements. Microstructure and mechanical properties of these alloys were investigated. A heat release process was identified during milling. This process is related to the reaction from pure elements to the intermetallic MoSi
2. The MoSi
2 alloys fabricated by MA-PDS process showed a very fine microstructure as compared to a sample sintered from commercial MoSi
2 powder. Significant hardness increase was found due to microstructure refinement for binary MoSi
2. Alloys made from powders milled in Air show higher hardness compared to those made with powders milled in Ar gas. This was attributed the oxides formed during milling process.
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