A mixture of elemental Co50Si50 powders was subjected to mechanical alloying (MA) at room temperature to prepare a CoSi thermoelectric compound. Consolidation of the Co50Si50 mechanically alloyed powders was performed in a spark plasma sintering (SPS) machine using graphite dies up to 800 °C and 1,000 °C under 50 MPa. We have revealed that a nanocrystalline CoSi thermoelectric compound can be produced from a mixture of elemental Co50Si50 powders by mechanical alloying after 20 hours. The average grain size estimated from a Hall plot of the CoSi intermetallic compound prepared after 40 hours of MA was 65 nm. The degree of shrinkage of the consolidated samples during SPS became significant at about 450 °C. All of the compact bodies had a high relative density of more than 94 % with a metallic glare on the surface. X-ray diffraction data showed that the SPS compact produced by sintering mechanically alloyed powders for 40-hours up to 800 °C consisted of only nanocrystalline CoSi with a grain size of 110 nm.

The mechanical alloying effect has been studied on the three Cu-based alloy systems with a positive heat of mixing. The extended bcc solid solution has been formed in the Cu-V system and an amorphous phase in the Cu-Ta system. However, it is round that a mixture of nanocrystalline Cu and Mo Is formed in the Cu-Mo system. The neutron diffraction has been employed at a main tool to characterize the detailed amorphization process. The formation of an amorphous phase in Cu-Ta system can be understood by assuming that the smaller Cu atoms preferentially enter into the bcc Ta lattice during ball milling.