Mechanical alloying of Ti-Si powder mixture was performed by high-energy ball milling at ambient temperature (25 °C). The structural and compositional evolutions during the mechanical alloying process were investigated by X-ray diffraction, energy dispersive spectroscopy, scanning electron microscopy and transmission electron microscopy. Results showed, that the crystallite size of Ti and Si decreased with increasing milling time and the steady-state crystallite size was between 5 and 15nm. The mechanically alloyed Ti-Si powder was predominantly nanocrystalline with traces of the remnant amorphous phase. It was found that a significant increase in solid solubility of Si in Ti was achieved by mechanical alloying. Interdiffusion between the two elements occurred during milling and the dissolution of Si in Ti was obtained after 60 h milling, forming Ti(Si) solid solution. The lattice parameter ratio c/a and the unit cell volume of h.c.p. Ti(Si) were found to decrease with increasing milling time, indicating that the shrinkage of Ti lattice was caused by diffusion of Si atoms into Ti. © 2004 Elsevier B.V. All rights reserved.