A laboratory process for preparation of Ni-Al intermetallic layers with definite phase composition has been developed in order to obtain protective coatings for use in hydrogen containing or hydrogen producing gas mixtures. Magnetron sputtering and electron beam evaporation, followed by heat treatment have been used for coating formation. Aluminum layers deposited on nickel supports were annealed in vacuum for 1-5 hours at 573-973 K. Coatings on powder, granules and carbon fibers have been also obtained by magnetron sputtering using composite Ni-Al targets. Structure and composition of layers have been investigated by XRD, XPS, electron and optical microscopy. The interaction of hydrogen sulfide with the coated samples have been studied. Coating surface structure and morphology depends on deposition and annealing conditions. These parameters also considerably influence the coated material＇s resistance to a hydrogen-containing atmosphere.