In this research, the microstructural and phase evolutions during mechanical alloying (MA) and subsequent heat treatment of Cu–Ti powder mixture are investigated through x-ray diffraction, scanning electron microscopy, transmission electron microscopy and micro-hardness measurements. The obtained experimental results demonstrated that after an optimumMAtime of 30 h, TiCu intermetallic compound was achieved with a mean grain size of≈8 nmand a high micro-hardness value of≈634 Hv. Annealing the milled powder at different temperatures resulted in formation of major TiCu and Ti2Cu3, and minor Ti2Cu and Cu4Ti nanocrystalline phases, release of internal strain, and coarsening of grains. The amount of TiCu phase and the grain size increased with increase of the annealing temperature. Micro-hardness value of≈765 Hv was recorded when the milled TiCu powder was annealed at 850 °C. This superior high micro-hardness value can be attributed to formation of higher amount of TiCu phase.
