Experimental study of methods for obtaining nanocrystalline molybdenum- and copper-based materials on from two independent crucibles (UE-187 device) on a stationary and rotating substrate has been done. The interaction of the separating layer with condensed Cu–Mo materials was investigated. The influence of technological factors (substrate material, surface roughness, composition and thickness of the separating layer, temperature of the substrate, change of the vacuum, evaporation rate of starting materials) on the mechanical properties of Cu–Mo condensed materials (with Mo from 0 to 46.5% wt.) was analysed. As found, in materials with a Mo more than 14% wt. and temperature of the substrate 700°C, strength is a dramatic decrease due to the formation of pores. Increasing the temperature of the substrate to 900°C allowed obtaining condensed composite Cu–Mo materials with a refractory phase up to 45% wt. As established, the regularities of formation of the technological layer of Cu–Mo condensate depend on the thickness of the separating layer of calcium fluoride. Due to the determination of mechanical characteristics of condensed composite materials obtained on rotating substrates with different surface roughness, it was found that a decrease of the roughness of the substrates leads to an increase in the ultimate tensile strength and elongation. As established, structural defects in the form of rods formed on micro-droplets ejected from the evaporator are the cause of reduced strength and ductility of condensed composite materials.