Porous Ni3Al intermetallic nano-compound was successfully prepared by a chemical method at 600 degrees C in a LiCl-CaH2 system. The prepared powder had a crystal structure completely identical to Ni3Al phase with a porous network structure formed by interconnected nanoparticles. The BET surface areas were as high as 13.1-13.6m(2)/g, corresponding to the estimated particle sizes of 59.0-61.3 nm. The surface areas were higher than previous reports (0.1-4.5m(2)/g) obtained by conventional physical methods.