This paper presents the results of a study of the oxidation behavior of NiAl produced by gel combustion synthesis calcined at two different temperatures. The objective is to compare the oxide growth rates, oxide scale composition, morphology and elemental composition of the sample powder subjected to isothermal oxidation and calcined at 1050 °C and 1300 °C for 1, 2, 4 and 10 hours by means of mass gain measurements, X-ray diffraction (XRD), field emission scanning electron microsocopy (FESEM) and energy-dispersive spectrometry (EDX) in order to investigate the reliability of the gel combustion synthesis method and evaluate the effect of calcination temperature on the oxidation behaviour of the powder. It was found that for the sample calcined at 1300°C the sample was made up mainly of metastable and stable alumina before oxidation and stable alpha alumina after oxidation whereas for the powder calcined at 1050°C the sample was mainly composed of detrimental mixed oxides before and after oxidation. Overall findings indicate that the oxidation behavior of the powder calcined at 1300°C is more protective compared to the powder calcined at 1050°C.