The non-equilibrium (Ti,Ni)C solid-solution phase was prepared by mechanical milling of a Ti-Ni alloy/graphite mixture. The formation of the non-equilibrium (Ti,Ni)C solid solution was confirmed by X-ray diffraction. The (Ti,Ni)C solid-solution phase was found to decompose into TiC and finely dispersed Ni during the heat treatment in vacuum obviously due to the thermal instability of the non-equilibrium phase. The instability of the (Ti,Ni)C phase was clearly demonstrated by the consideration on the Gibbs free energy of formation of the phase. This new method allows the production of premixed TiC-Ni composite powder having a fine and uniform composition which may provide enhanced properties over the conventionally mixed TiC-Ni powder. (C) 2013 Elsevier B.V. All rights reserved.