In this study, (Fe,Ti)(3)Al-Al2O3 nanocomposite was synthesized by mechanical alloying (MA) of Al-Ti-Fe2O3 powder mixture. Structural evolution and thermal analysis of powder particles during MA were studied by X-ray diffractometry (XRD) and differential thermal analysis (DTA). Kinetic analysis of Fe2O3-Al reaction was conducted using free model methods. The (Fe,Ti)(3)Al-Al2O3 nanocomposite was formed during MA via Fe2O3-Al thermite reaction. The Fe2O3-Al reaction appeared to occur in combustion mode and the formation of (Fe, Ti)(3)Al-Al2O3 nanocomposite occurred in two consecutive stages. In the first stage, Al2O3 and in the second stage, (Fe,Ti)(3)Al phases were formed. Kinetic analysis revealed that for ball milled powders the reaction of Fe2O3 with Al can take place below Al melting temperature with a different reaction path. (C) 2013 Elsevier B.V. All rights reserved.