Multilayer thin films Al/Cu/Fe were deposited in different sequences by sputtering in a triode system. After the deposition the samples were annealed in an inert atmosphere at temperatures up to 600 degreesC in order to obtain a homogeneous film with the desirable composition Al62Cu25Fe13. This was achieved by proper thickness ratio of individual films and adequate annealing temperature. AES depth profiling was used to follow the diffusion processes in the film. Using XRD the binary AlCu3 and ternary beta-AlCuFe phases were detected, depending on the annealing temperature. The evolution of these phases is accompanied by a rise of both microhardness and electrical resistivity. (C) 2003 Elsevier B.V. All rights reserved.