In this work, an Al/Fe3Al core-shell nanoparticle was obtained by heat treatment of a precursor in high purity of argon. The precursor, with Fe(CO)(5) and nano Al as raw materials, was synthesized simply by a chemical liquid deposition method. The evolution of the phase and morphology during the heat-treatment has been carefully studied by XRD and TEM. The results indicate that the precursor transformed to core-shell structure of Fe3Al intermetallic nanoparticle. The formation of the Fe3Al intermetallic nanoparticle was explored by DSC test, which reveals that the formation temperature of the nanoparticle is around 587 degrees C. Moreover, the TG-DSC measurements from 50 degrees C to 1000 degrees C in compressed air (20% O-2 and 80% N-2) reveal that the heat-treated powder of the precursor remains thermal stability in relatively low temperature but becomes concentrated combustion in elevated temperature. (C) 2013 The Society of Powder Technology Japan. Published by Elsevier B. V. and The Society of Powder Technology Japan. All rights reserved.