Nanocomposite SiO₂CuO_x materials (films and powders) synthesized by sol-gel method have been studied. X-ray absorption spectroscopy and photoelectron spectroscopy has been applied to investigate the phase composition and oxidation states of the copper. The CuL_2,3 NEXAFS experimental spectra of the samples have been compared with X-ray photoelectronic films spectra. The samples synthesised with 300 and 500 °C heat treatment showed the presence of copper compounds corresponding to the CuO phase. The CuO and Cu₂O phases, as well as the CuSiO₃ double oxide phase have been found in the films.

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