The reduction and carburization behavior of NiO–WO 3 mixtures by CO was studied using thermogravimetric and differential thermal analysis techniques (TGA–DTA) with the aim of preparing homogenous Ni–WC composite powders. Based on the TGA–DTA results and characterization of the reaction products using XRD and SEM, the following reaction path is suggested. Reduction of NiO with CO begins at 550°C, followed by reduction of WO 3 to first WO 2 by CO, and then to W by carbon. The generation of W was accompanied by its carburization through C and CO. The reactions were near completion at 850°C, producing clusters of Ni–WC in the few micrometer range. Increasing the Ni content of the mixture resulted in greater carbon deposition, also appeared to widen the temperature range for the reactions.