High-energy mechanical alloying (MA) of a micrometer-scaled W and TiC powder mixture was performed to prepare TiC/W nanocomposites. X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), transmission electron microscope (TEM), and laser particle size analysis were used to study the morphological change and microstructural evolution occurred during MA process. It showed that the powder particles experienced a continuous refinement during 0-35 h milling; on increasing the applied milling time up to 45 h, the particles had a tendency to coarsen. The 35 h milled powder had a considerably refined particle morphology, showing a narrow size distribution (D-25 = 0.47 mu m, D-50 = 0.61 mu m, D-75 = 0.74 mu m, and D-90 = 0.86 mu m) and a significantly elevated specific surface area of 4154.86 m(2)/kg. The TEM results revealed that the particles of 35 h milled product consisted of a large number of ultrafine crystallites of W and TiC with sizes less than 20 nm and the nanometer-sized TiC particulates were dispersed uniformly throughout the W matrix. The analysis of XRD spectra by Scherrer equation indicated that the average crystallite sizes of the W and TiC constituents in the 35 h milled powder were 8.5 nm and 13.6 nm, respectively, showing a good agreement with the experimental results. On further increasing the milling time up to 45 h, the partial amorphization of W constituent occurred in the milled powder. Formation mechanisms and theoretical basis for microstructural development and phase change in the milled powders were elucidated. (C) 2013 Elsevier B.V. All rights reserved.