The silica nanolayer with different thickness was coated on the spherical cobalt nanoparticles (an average diameter of 67 nm) to form core-shell structure by the controlled hydrolysis and condensation of tetraethyl orthosilicate (TEOS). This coating process was based on the use of silane coupling agent 3-mercaptopropyltrimethoxysilane (HS-(CH2)(3)Si(OCH3)(3), MPTS) as a primer to render the cobalt surface vitreophilic, thus rendering cobalt surface compatible with silica. The control over the silica coating layer thickness can be achieved by varying the reaction time. The cobalt nanoparticles and the cobalt coated with silica shell were confirmed by transmission electron microscopy (TEM). X-ray photoelectron spectroscopy (XPS) was used to gain insight into the way in which the MPTS is bound to the surface of the cobalt nanoparticles. Result of the thermogravimetric analysis (TGA) and differential thermal analysis (DTA) indicate that the thermal stability of cobalt/silica is better than that of pure cobalt nanoparticles. Magnetic properties of these powders have been evaluated. These cobalt/silica core-shell nanoparticles can be utilized as precursors for making property-tunable magnetic nanoparticles, thin films, and multilayered core-shell structure nanocomposites. (c) 2006 Elsevier B.V. All rights reserved.