Mechanical alloying (MA) of Ti-37.5mol%Si composition powder mixture (stoichiometric composition of Ti₅Si₃ intermetallic compound) and synthesis of Ti-silicides by milling and heat treatment of MAed powders were investigated. The formation of TiSi and TiSi₂ phase were observed by milling over 540ks, but stoichiometric phase, Ti₅Si₃, was not formed only by milling. Fully MAed powder (more than 1800ks) changed to almost Ti₅Si₃ single phase after DTA runs up to 1173K. On the other hand, in the case of short period MAed powders, TiSi and TiSi₂ were also formed during DTA runs in addition to the Ti₅Si₃.
We tried to make a dense compact using the vacuum hot pressing technique. Relative density of hot pressed compact was 99.7% of theoretical density. The hot pressed compact showed high micro-Vickers hardness more than HV 1300 and K_IC value of 1.46MPa⋅m^1/2. Fracture toughness of the compact exceeded the value of arc melted material, 1.19MPa.m^1/2.