This paper describes the study of the structural properties of the alloy layers prepared by two different, impulsively working PAPVD methods: the Pulsed Magnetron Sputtering (PMS) and the Impulse Plasma Deposition (IPD). The Fe-Cu alloy layers were synthesized. The results of our investigation revealed a nanocrystalline structure of the layers. The differences in the phase composition of the Fe-Cu alloy layers produced by these two methods were observed. The synthesis of the Fe-Cu layers by using the Pulsed Magnetron Sputtering method resulted in obtaining the two-phase, polycrystalline structures (fcc-Cu and bcc-Fe). In this case the clear evidence of mixing between the iron and copper atoms was not observed. The Fe-Cu layers deposited by the Impulse Plasma Deposition method were characterized by the nonequilibrium phase composition -the presence of one-phase supersaturated solid solution (fcc-Cu(Fe) or bcc-Fe(Cu)) was formed in immiscible systems. These results suggest a short-distance diffusion between the neighboring nanoparticles of the two metals (Cu and Fe) occurring during the IPD layers growth. (C) 2013 Elsevier B.V. All rights reserved.