Аннотация:Au, Fe, and AuFe nanoparticles were obtained by metal vapor synthesis using acetone as the dispersion medium. The composition and electronic structure of the particles were studied by TEM, SEM, XPS, XANES, and EXAFS. The Au and Fe particles with average diameters of 5.3 and 1.8 nm, respectively, were obtained. According to X-ray diagnostic methods, gold was in the Au(0) state, while iron existed as mixture of non-stoichiometric oxides with states close to Fe2+ and Fe3+. Bimetallic nanoparticles were solid solutions with a disordered structure and Au–Fe–O and Au–O–Fe bonds. A carbon-containing shell wasdetected for all types of metal particles. The obtained materials may be promising for the development of improved antimicrobial agents and new methods for treating cancer diseases.