In this study, NiAl–Al2O3-WC nanocomposite has been synthesized from the Al–NiO–W–C powder mixture by mechanical alloying and subsequent heat treatment. Phase development and structural changes were studied by X-ray diffraction technique, feld-emission gun scanning electron microscopy, and transmission electron microscopy. XRD results showed that NiO was disappeared after 20 h milling and NiAl and W2C phases were formed. By the increase of milling time, no phase development was observed. So for access to desired compounds, 40 h milled powder thermally treated at 1200 °C for 3 h, and XRD and TEM results confrmed the formation of NiAl-WC-Al2O3 nanocomposite.