The preparation of titanium carbide/aluminurn oxide (TiC/Al2O3,) nanocomposite powders from a mixture of titanium, carbon, and Al2O3 powders via a high-energy ball milling process and subsequent heat treatment was investigated. The microstructure development of the powder mixtures was monitored by X-ray diffraction and transmission electron microscopy. The ball milling of an elemental carbon, titanium, and Al2O3 powder mixture at ambient temperature resulted in the formation of TiC within 15 h of milling. With further milling of up to 25 h, the resulting powder mixture was composed of nanosized TiC particles and nanocrystalline carbon, titanium, and Al2O3. The nanocrystalline titanium and carbon were transformed into nanosized TiC particles after subsequent heat treatment. The final product was composed of nanosized TiC and microcrystalline Al2O3. Most of the nanosized TiC particles were located within Al2O3 grains.