A modified sol-gel technique was used to synthesize nanocomposites of Ni:SiO2 which resulted in Ni nanoparticles embedded in a SiO2 amorphous matrix. Transmission electron microscopy TEM analysis were performed to study the structure and morphology of the magnetic powders. The Ni particles were found to have a good dispersion and a controlled particle size distribution, with average particle radius of ∼ 3 nm. A detailed characterization of the magnetic properties was done through magnetization measurements M(T,H) in applied magnetic fields up to ± 7 T and for temperatures ranging from 2 to 300 K. The superparamagnetic (SPM) behavior of these metallic nanoparticles was inferred from the temperature dependence of the magnetization. The blocking temperature TB, as low as 20 K, was found to be dependent on Ni concentration, increasing with increasing Ni content. The SPM behavior above the blocking temperature TB was confirmed by the collapse of M/MS vs. H/T data in universal curves. These curves were fitted to a log-normal weighted Langevin function allowing us to determine the distribution of magnetic moments. Using the fitted magnetic moments and the Ni saturation magnetization, the radii of spherical particles were determined to be close to ∼ 3 nm, in excellent agreement with TEM analysis. Also, magnetic hysteresis loops were found to be symmetric along the field axis with no shift via exchange bias, suggesting that Ni particles are free from an oxide layer. In addition, for the most diluted samples, the magnetic behavior of these Ni nanoparticles is in excellent agreement with the predictions of randomly oriented and noninteracting magnetic particles. This was confirmed by the temperature dependence of the coercivity field that obeys the relation HC(T) = HC0 [1-(T/TB)1/2] below TB with HC0 ∼ 780 Oe.