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Production of clean hydrogen from thermal decomposition of methane was studied over impregnated 30%Fe/Al2O3 catalysts in a micro-activity fixed-bed reactor. The reactant gases comprising CH4 and N2 in the ratio of 1.5 to 1 were passed through reactor at a flow rate of 25 mL/min. Moreover, effect of calcination was investigated as well. The catalytic activity results indicated that calcination temperature had a significant impact on the performance of 30%Fe/Al2O3 catalyst. The catalyst calcined at 450°C, having CH4 conversion as well as H2 yield over 70%, showed better activity as compared to all other calcination temperatures.