In-situ synthesis of WC-Al2O3 composite by milling and its subsequent heat treatment were investigated. Mixtures of Al,W, and Cwith stoichiometric ratio ofW3AlC2 were ball milled up to 20 h. Then, the 20-hour ball milled powder was heat treated at different temperatures of 900 and 1200 °C. The reaction path was investigated by Xray diffractometry (XRD). The particle size and microstructure of powders after milling was investigated by field emission scanning electron microscope (FESEM) equipped with energy-dispersive spectroscopy (EDS). Also, in order to analyze the heating behavior of 20 h ball milled powder mixture during heat treatment, simultaneous thermal analysis (STA) was used. The results showed that after milling for 20 h, the reactants reacted together and newphases includingW2C and (W,Al)C1 − xwere formed. After heat treatment, the semi-stable compounds synthesized at the milling stage, were transferred to more stable compounds including WC and Al2O3.