Samples of 316L austenitic steel were submitted to a thermochemical treatment which implies surface diffusion of Al and Ti. The technique of pack cementation with NH4Cl as activator was employed. The powder mixture was made of aluminium, titanium, aluminium oxide and ammonium chloride. The same ratio of Al : Ti = 1 : 5 was used in all experiments. The variables were temperature and time. As a function of these parameters, diffusion layers of different thicknesses were obtained. The samples were analyzed by optical microscopy, scanning electron microscopy (SEM) and energy dispersive X-ray microanalysis (EDX), X-ray diffraction and Vickers microhardness trials. All layers were formed by diffusion with reaction and present two zones with different structures and compositions and therefore different properties. The Ti3NiAl2N compound was identified by X-ray diffraction. The presence of this compound in the diffusion coatings increases the superficial hardness of the samples.