In this paper the feasibility of NbAl3/Al2O3 nanocomposite formation through mechanochemical reaction between Al and Nb2O5 and the effect of mechanical activation on the kinetic and reaction mechanism were investigated. Structural and phase evolution during mechanical alloying were studied by employing transmission electron microscopy (TEM), X-ray diffraction (XRD) and differential thermal analysis (DTA) techniques. It was found from the results that the reduction of Nb2O5 by Al takes place in an explosive mode and after 450 min of mechanical alloying leading to the formation a microstructure consisting of NbAl3 matrix and nanocrystalline Al2O3 particles. The results also showed that heating the as-blended powder mixture of Nb2O5 and Al, leads to the formation of NbAl3/Al2O3 composite through two exothermic reaction; A thermite reaction at 880oC followed by the synthesis of NbAl3 intermetallic at 944 oC. The mechanical activation of Nb2O5 and Al powder for 5h decreased the formation temperature of NbAl3/Al2O3 from 944oC to 625oC. Five isoconversional methods, of Kissinger-Akahira-Sunose, Tang, Flynn-Wall-Ozawa, Starink and Friedman were used to determine the activation energy, Ea, for NbAl3/Al2O3 formation reaction and its variation with conversion degreea. The results showed that these methods lead to similar or comparable values of Eα.