The compounds that can be used as a separating layer in the formation of composites obtained by the electron-beam evaporation-condensation method were analysed. It is shown that a transitional technological layer is formed between the separation layer and the condensate, the composition and structure of which depends on the separation layer thickness. Large values of the separation layer thickness, cracks are formed, which are transformed into a technological layer and into condensate and reduce the mechanical properties of condensates. Conducted researches confirmed the formation mechanism of Cu–Mo, Cu–W, Cu–Fe, Cu–Ni composite materials condensed from the vapor phase according to the scheme: steam → liquid → spheroidal particles → nuclei on the technological layer → attachment of particles to nuclei.