Nickel silicides (Si, NiSi and NiSi) have been synthesized by mechanical alloying (MA) of Ni-27.9at.9at%Si, Ni-33.3at% and Ni-50.0at% powder mixtures, respectively. From in situ thermal analysis, eash citical milling period for the formation of the three phases was observed to be 40.2, 34.9 and 57.5 min, at which there was a rapid increase in temperature. This indicates that rapid, self-propagating high-temperature synthesis (SHS) reactions were observed to produce the three phases during room-temperature high-energy ball milling of elemental powders. Each Ni silicide, Ni and Si, however, coexisted for an extended milling time even after the critical milling period. The powders mechanically alloyed after the critical period showed the rapid increase in microhardness. The Hv values were found to be higher than 1000kgf/mm. The formation of nickel silicides by mechanical alloying and the relevant reaction rates appeared to be influenced by the critical milling period and the heat of formation of the products involved (Si-43.1kJ/mol.at., NiSi-47.6kJ/mol.at., NiSi-42.4kJ/mol.at).

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