Catalysts based on mixed oxide of type NiaFe1-aO4 (a=0,5 a 0,9) were prepared by coprecipitation using potassium hydroxide 1M KOH (pH variable ~2 to 12) as precipitating agent for oxidative dehydrogenation (ODH) of ethane and were characterized by X-ray diffraction (XRD), sorption of N2 (BET’s method), temperature programmed reduction with hydrogen (TPR-H2), temperature programmed desorption with ammonia (TPD-NH3) and laser Raman spectroscopy (LRS). The ODH of ethane has been performed in a fixed-bed quartz reactor for a constant W/F (contact time) ratio of 0.48 g.s/mL. The introduction of Fe+3 (0.64 Å) into NiO (0.72 Å) framework allowed to decrease initial crystal parameter cell of the catalysts Ni0.9Fe0.1Ox and Ni0.8Fe0.2Ox, however, the introduction of Ni2+ into NiFe2O4 the intensity decreased nickel oxide which was verified by XRD analysis and led to a drastic improvement of specific surface (BET’s method), lower pore size (BJH’s method) and crystallite (Scherrer’s equation), in relation with simple samples. For the activity determination of the activity of the catalysts as a function of temperature, the weight of the sample was 0.4 g and its particle size was 150m and the total flow was 50 mL/min. The catalytic activity of the NiaFe1-aOx mixed oxide catalysts in the ODH reaction was explored under steady state conditions between 250-400°C and C2H6/O2=1/1 ratio. Furthermore, the ethane/ethene conversion and selectivity to the reaction were calculated on a carbon basis. Closure of the carbon mass balance was 5%. The selectivity improved drastically at temperatures ranging from 250 to 400°C, taking into count that CO2 and ethylene were the final products. The maximum selectivity to ethylene was 84% which was obtained with Ni0.8Fe0.2Ox at 300 ºC as a probably consequence of multifactor contribution of higher surface area in relation to simple samples, major tendency to decrease the reduction temperature with the enrichment of nickel in the mixed composition and the presence of spinel species in crystal structures which were detected by LRS.