The present study is about the synthesis of Al2O3–WC nano composite powders obtained through mechanochemical process. Generally, the mode of reaction inWO3, Al and C mixture is MSR (mechanically induced self-propagating reaction). In order to elimination of undesirable W2C, separation of reactions and conducting the heat with time intervals were used. Hence, at the initial stage WO3 and Al powders milled in a high-energy ball mill for 1 h. Subsequently, 1 mol C is added to the milled powders and milled stepwise. Al2O3–WC Composite is obtained after 20h milling. To investigate morphological aspects of powder’s surface, Scanning Electron Microscopy (SEM) analysis is utilized. In addition, Powder samples were characterized by X-ray diffraction (XRD) and Energy-dispersive X-ray Spectroscopy (EDX). Also the crystallite size of the produced nano composite was calculated According to Williamson–Hall method to about 31nm.