In this research, the formation of TiC nanopowder was investigated by mechanochemical reaction of titanium and graphite starting materials during milling. The evolutions in temperature and pressure were evaluated using thermal-pressure sensor during milling. Phase transformation, grain size, strain, lattice parameter, introduction of Fe impurity, morphology of powders and particles size distribution during milling were examined using different analysis techniques including XRD. Rietveld refinement, ICP, SEM, TEM, Zeta sizer and BET. Nanocrystalline TiC was obtained by an abrupt increase in the temperature and pressure of the vial after a short milling time that confirmed mechanochemical mechanism by an exothermic reaction. Longer milling times resulted in decreasing of TiC particles size toward nanosize scale along with increasing of Fe impurity. (C) 2011 Elsevier B.V. All rights reserved.