Sol-gel derived silica (SiO2) films doped with nickel oxide (NiO) nanocrystals were fabricated. A bifunctional ligand was used, bearing amine groups capable of coordinating the nickel ions and hydrolysable siloxane groups for anchoring the metal complex moiety to the silicate matrix. Nickel oxide nanocrystals precipitated at 500degreesC while the film was still porous. The nanocomposite films showed a reversible change in the optical transmittance in the VIS-NIR range when exposed to carbon monoxide gas. The effects of residual porosity, testing temperature, and carbon monoxide gas concentration on optical transmittance were studied.