Ti3AlC2/Al2O3 nanopowders were synthesized by the combination of mechanically-induce self-propagating reaction (MSR) of Ti, C, Al and TiO2 powder mixtures and subsequently heat treatment. Effects of high energy milling and heat treatment temperatures on the phase transformation were investigated in detail. X-ray diffraction (XRD) was used to characterize the powders of milled and annealed, respectively. The morphology and microstructure of as fabricated products were also studied by scanning electron microscopy (SEM) equipped with energy-dispersive spectroscopy (EDS). Results show that TiC, TixAly and Al2O3 transitional phases were formed when the initial powder mixtures were milled for 24 h. The desired Ti3AlC2/Al2O3 nanopowders with high purity were obtained when annealed the as-milled powders at 1100 degrees C. SEM image confirmed that the as fabricated Ti3AlC2/Al2O3 particles has nanocrystalline layered structural matrix of Ti3AlC2, and the second phase of nanosized Al2O3 disperses uniformly in the Ti3AlC2 matrix. (c) 2010 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.