The SiO2:Fe films on Si substrates were produced by sol-gel and spinning techniques. Hybrid organic-inorganic precursor (tetraethoxysilane-FeCl3) and organic alkoxide precursor modified from Fe acetate were used. The Fe nanoparticles have been formed by various technological procedures. The structural, magnetic and optical characteristics of (SiO2:Fe) / Si samples depending on technology of sample preparation were examined. The size of Fe nanoparticles was shown to be controlled by precursor preparation procedure. It was found that Fe-containing nanocrystals of average size ∼40 nm were formed by "one-pot" technique from the mixture of solutions containing Fe salts and freshly prepared colloidal tetraethoxysilane (TEOS). In contrast, in the "two-pots" procedure, the components of precursor were prepared non-simultaneously and the structurized TEOS sol was used. In the latter case, Fe nanoparticles were distributed in size over a larger range with a mean value at ∼25 nm. It was hence concluded that precursor-controlled formation of Fe nanoparticles can be achieved using different sol-gel technological procedures.