Abstract.The combination of energy dispersive spectroscopy (EDS) and electron backscatter diffraction (EBSD) techniques in scanning electron microscope was employed to characterize the reacted interface between Ti matrix and AlN particles. Due to the high localization of EDS and EBSD, representative measurements of chemical composition and reliable determination of the crystal structure were possible for each phase in the reaction zone with complex morphology. The TiN1x (cubic, NaCl type), Ti3AlN (cubic, perovskite type) and Ti-rich Ti3 Al (hexagonal, Ni3Sn type) phases were identified in the reaction zone after annealing at 1100C. EDS+EBSD combination is an efficient tool for phase analysis at the interface in reactive multicomponent systems.