For the first time nanoporous Zn and Ni particles were synthesized in dimethyl sulphoxide (DMSO) by a sonoelectrochemical method. The as-prepared samples were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen sorption. It was found that these nanopores were produced by the aggregation and/or melting of primary nanoparticles of about 45 nm in size under ultrasound irradiation after electrochemical reduction of metal ions. The utilization of nonaqueous solvent prevented the oxidation of these active metal nanoparticles, while the presence of poly-(vinylpyrrolidone) could inhibit the growth of the nanoparticles. This study provides a general method to continuously prepare nanoporous active metal particles from inorganic metal salts with high yields. (c) 2007 Elsevier B.V. All rights reserved.