Nickel nanoparticles coated with zinc sulphide can form complex spherical with a core-shell structure. This coating process was based on mercaptoacetic acid (HSCH2COOH) as a primer to render the nickel Surface vitreophilic, thus it renders nickel surface compatible with ZnS. The morphology, structure, chemical composition, optical properties and magnetic properties of the product were investigated by using various techniques, including transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), photoluminescence (PL) spectroscope and vibrating sample magnetometer (VSM). It was found that the Ni/ZnS nanocomposites exhibited both magnetic and photoluminescent properties. (c) 2008 Elsevier B.V. All rights reserved.