Ni-Ferrite (NiFe₂O₄) was prepared as a basic metal oxide for a solar hydrogen production cycle consisting of a methane reduction step and a water-splitting step. All steps were performed at relatively low temperatures (below 1073 K). In the CH₄-reduction step, it was confirmed that CH₄ reduction of the prepared Ni-ferrite progressed through two reaction regions with an increase of reaction time. In one, CH₄ reacted with oxygen discharged from Ni-ferrite (region 1); in the other, the methane self-decomposition occurred (region 2). The water splitting step was performed using the reduced Ni-ferrite after the CH₄ reduction step in the two regions. In the water splitting step after the CH₄ reduction step (region 1), CO and CO₂ gas were not detected. The maximum H₂ production rate was about 3.3 mL/min g-metal-oxide at 10 min. The H₂ production rate in the water splitting step after the CH₄ reduction step (region 2) was about 3.3 mL/min g-metal-oxide at any reaction time, We confirmed from the XRD patterns that the phase of the prepared Ni-bearing ferrites was changed in each reaction step and that the phase after the water splitting step returned to the phase before the methane reduction step.