A Ti3SnC2–Al2O3 composite was produced by mechanical alloying and subsequent differential thermal analysis (DTA) of 3TiO2/4Al/1Sn/2C powder mixture. The starting powder was milled up to 40 h. To determine the formation mechanism, a 40 h milled powder was evaluated by DTA. X-ray diffraction was used to evaluate powder samples. Later, morphological and microstructural characteristics of the samples were obtained by highresolution scanning electron microscopy. Followed by milling, the patterns of X-ray diffraction showed a homogeneous distribution of fine reactant powders without new phases that after 40 h of milling. According to the DTA, several thermal events occurred during the 40 h of milling and Ti3SnC2/Al2O3 was formed, consequently. The formation mechanism of Ti3SnC2/Al2O3 composite consisted of Sn melting, Al melting, TiO2 reduction, Ti5Sn3 and TiC formation, and reaction among Ti, C, Ti5Sn3 and TiC, as well as Ti3SnC2 formation
