The paper presents the results of investigations into the structure and properties of Ni-Al diffusion layers produced on INCONEL 100 by Chemical Vapour Deposition (CVD). The process was carried out in aluminium chloride (AlCl3) mixed with hydrogen atmosphere. The as-deposited layers were subjected to thermal treatment in vacuum to optimize their adhesion, hardness and temperature-resistance. Microstructural characterization of the coatings was carried out by scanning electron microscopy (SEM) The chemical composition was measured via EDS and the phase content was investigated by X-ray diffraction XRD. The resistance to high temperature of the coatings at atmospheric pressure was tested by applying 24-hours cycles at 950 °C. Scratch-tests provided data on the microhardness and adhesion of the coatings. The results indicate that the layers produced on the INCONEL 100 exhibit a very good adhesion combined with exceptional corrosion resistance at high temperatures.