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The effect of method preparation on the activity of Fe2O3-NiO/γ-Al2O3 catalyst was investigated in process decomposition of methane. Fe2O3-NiO/γ-Al2O3 catalyst was prepared by impregnation and solution combustion methods. The samples were characterized by X-ray phase analysis (XRD), temperature-programmed hydrogen reduction (TPR-H2), BET and Raman spectroscopy. It has been shown that the method of preparation plays an important role in regulating the textural and morphological properties of catalysts and provides a difference in their catalytic activity. The synthesis of the Fe2O3-NiO/γ-Al2O3 catalyst by the solution combustion method, in comparison with the capillary impregnation method, leads to the formation of a large amount of FeNi and FeAl2O4 solid solutions, which ensured good catalytic activity at high temperatures. The Fe2O3-NiO/γ-Al2O3 catalyst synthesized by the solution combustion method demonstrated good activity with a hydrogen yield of 52% within 150 min of the reaction without any deactivation. According to the results of Raman spectroscopy, graphene-like carbon was obtained on the surface of the catalysts. On the catalyst of Fe2O3-NiO/γ-Al2O3 (СI) synthesized by capillary impregnation, 4‒5 layer graphene on Fe2O3-NiO/γ-Al2O3 (SC)-6-7 layer graphene is formed.