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The metal vapor synthesis (MVS) is an efficient means of purposeful synthesis of nanosized metallic particles as well as their derived composites. The modification of polymers with metal nanoparticles gives rise to several attractive functional properties, e.g., magnetic, catalytic, antibacterial ones. New hybrid materials based on copper nanoparticles stabilized in a ulitmately biocompatible chitosan matrix were prepared via MVS. Transmission electron microscopy shows that the particles have predominantly spherical form, polydisperse character, the mean diameter about 2-3 nm and a rather uniform distribution in the chitosan matrice. X-ray Photoelectron spectroscopy analysis of Cu-carrying chitosan powder obtained by impregnation of chitosan powder with Cu-acetone organosol indicated two oxidized copper states on the surface. Cu2+ и Cu+ concentrations (at. %) calculated from the spectra were 10.7 and 3.6%, respectively. The antifungal activity of the copper-chitosane nanocomposites (Cu@Chit NCs) against the linear growth of Fusarium solani and Macrophomina phaseolina was evaluated in vitro and their effects on hyphal growth were evaluated. The structure of the materials was studied using X-ray and synchrotron techniques, viz., X-ray diffraction, X-ray absorption spectroscopy XANES/EXAFS. The results show that the Cu@Chit NCs synthesized via MVS with acetone as intermediate nanoparticle stabilizer are highly effecient in inhibiting growth of Fusarium solani fungal hyphae.