Nanoparticles of NiO, Ni or NiS have been obtained by solvothermal decomposition of different molecular precursors. The influence of several parameters, such as temperature, reaction time, solvent or capping agent used, in the nature and size of the obtained nanoparticle has been studied. The characterization by XRD and TEM techniques indicates that the nanoparticles of NiO exhibit average sizes of 3-8 nm, while those of Ni are in the 30-40 nm range. This difference in size has been attributed to the presence of molecules of the capping agent (n-octylamine or oleic acid) that surround the NiO nanoparticles but were not present in the nickel ones. The capping agent is, thus, preventing the aggregation of the smallest nanoparticles. The use of either a S-donor capping agent (4-mercaptopyridine) or a precursor having S-donor ligands (diethyldithiocarbamate) have led to the formation of NiS with average sizes around 35 nm. The magnetic properties of the nanoparticles have been studied, showing superparamagnetism and magnetic hysteresis below the blocking temperature, which, in time, is dependent of the particle size.