Possibility of layer-by-layer synthesis by colloidal layering of Sb ₂S₃-SiO₂ nanocomposite layers from colloid solutions of {[H _x Sb₂S₅] ^m -}mNa⁺ and SiO₂ was studied. The composition of the layers synthesized was examined by Raman spectroscopy, transmission spectroscopy in the UV and visible spectral ranges, energy-dispersion micro analysis, and scanning electron microscopy.