Nanometer nickel powders have been prepared using the polyol method with NaOH, Ni(NO3)(2)center dot 6H(2)O, ethylene glycol (EG), and polyvinylpyrrolidone (PVP) as raw materials. The thermodynamics of the reaction system was studied, and the E-pH diagram of Ni-EG-H2O was plotted. The oxidation products of EG were predicted from the E-pH diagram, and CO32- in alkaline solutions was identified as the product through the IR spectrum and CaCO3 sediment. Field-emission scanning electron micrograph (FESEM) showed that spherical nanometer nickel powders were obtained. (c) 2006 Elsevier Ltd. All rights reserved.