For the first time conditions were determined for the synthesis of Cu _x SiO_2+x·nH₂O nanostructured layers by consecutive adsorption of copper ammine cations and adagulation of colloidal SiO₂ particles and also for the synthesis of xCuS-SiO ₂·nH₂O nanocomposite layers by consecutive surface adsorption of copper cations and HS^- anions. These layers were studied by means of UV and visible transmission spectroscopy, X-ray spectral microanalysis, and scanning electron microscopy. Schemes of the surface reactions were constructed on the basis of this experimental material.