Abstract: The thermochemical CO₂ splitting activity of NiFe₂O₄ and NiFe₂O₄/ZrO₂ prepared by the conventional co-precipitation method was investigated with thermogravimetric analysis (TGA) technique. Significant sintering was observed over the two samples during cyclic reactions because of the high reaction temperature. This would lead to an incomplete re-oxidation of the reduced sample in the CO₂ splitting reaction. Introduction of ZrO₂ could greatly enhance the thermal stability of NiFe₂O₄, and hence, the cycling behavior in repeated cycles. The catalytic results of NiFe₂O₄/ZrO₂ for cyclic splitting of CO₂ in a high-temperature furnace indicate that CO productivity increased with the thermal reduction temperature, while the cycling stability severely decreased with the cyclic number.