Nickel aluminide powders were prepared by direct electrochemical reduction of solid mixture of NiO-NiAl2O4 (Ni:Al = 1:1 in mol) precursor in molten CaCl2 at 850 degrees C. The reduction process of the solid oxide cathode was investigated by analyzing the intermediate products using X-ray diffraction (XRD) and scanning electron microscopy (SEM). It reveals that nickel is preferentially reduced and it benefits to prevent aluminum leaving from the cathode. The products obtained at the constant cell voltage electrolysis of 3.0 V for more than 4 h were stoichiometric NiAl. The energy consumption could be as low as 6.1 kWh (kg-NiAl)(-1) based on the applied cell voltage and the consumed electrolysis charge. Furthermore, the NiAl powders were made into a dense rod by spark plasma sintering (SPS) technique. The corrosion behaviors of the NiAl rod in 0.5 mol L-1 NaCl aqueous solution at room temperature were investigated by polarization curve and ac impedance measurements. It was found that the NiAl rod had satisfactory anti-corrosion ability in the solution. (C) 2012 Elsevier BM. All rights reserved.