Hydrogen production by a 2-step water-splitting thermochemical cycle using metal oxides (ferrites) redox pairs and CH4 have been studied in this experiment. Reactions were performed in a two-step redox cycle in which the ferrites were reacted with CH4 at 700°C–800°C to produce CO, H2, and various reduced phases (reduction step); these were then reoxidized with water vapor to generate H2 in water-splitting step (oxidation step) at 600°C–700°C. The reduced forms of Ni-Fe2O3, Ni-FeO and Ni-Fe alloy from XRD, showed respectively different reactivity for H2 formation from H2O. These were oxidized to the ferrite phase to produce H2 in the water-splitting step at 600°C–700°C. In reduction reaction at 800°C, carbon deposition arise on surface of Ni-ferrite due to CH4 decomposition. This reduced phase containing carbon, which reacts with H2O at 600°C, produce H2, CO, and CO2. The amount of H2 evolved using reduced phase containing carbon was much than that of other phase.