Recebido em 3/9/04; aceito em 20/1/05; publicado na web em 30/6/05 SYNTHESIS AND CHARACTERIZATION OF Ni:SiO 2 NANOCOMPOSITES PROCESSED AS THIN FILMS. We have produced nanocomposite films of Ni:SiO 2 by an alternative polymeric precursor route. Films, with thickness of ~ 1000 nm, were characterized by several techniques including X-ray diffraction, scanning electron microscopy, atomic force microscopy, flame absorption atomic spectrometry, and dc magnetization. Results from the microstructural characterizations indicated that metallic Ni-nanoparticles with average diameter of ~ 3 nm are homogeneously distributed in an amorphous SiO 2 matrix. Magnetization measurements revealed a blocking temperature T B ~ 7 K for the most diluted sample and the absence of an exchange bias suggesting that Ni nanoparticles are free from an oxide layer.