Nanocomposite Ni(1-x)/(SiO2). soft magnetic materials were synthesized by a simple sol-gel combined hydrogen reduction method. The crystal structure of the particles was determined by X-ray diffraction (XRD). The shapes and sizes of the metal particles embedded in the SiO2 matrix were determined by transmission electron microscopy (TEM), and magnetic properties were measured by the vibrating samples magnetometer (VSM). The obtained nanocomposite material is composed of nanoparticles coated with a thin SiO2 layer, and with the content of the silicon increase, the thickness of the silica shells increase and the saturation magnetization decrease. The diameter of Ni particle in the sample is about 30-40 nm. The influence of the Ni content and preparation conditions on the microstructures and magnetic properties were discussed. (c) 2008 Elsevier BY. All rights reserved.