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In this study, ZnFe₂O₄ and ZnO-ZnFe₂O₄ catalysts were prepared using the glycine–nitrate process (GNP). The prepared ZnFe₂O₄ and ZnO-ZnFe₂O₄ catalyst powders were characterized using a scanning electron microscope, transmission electron microscope, XRD diffraction studies, and selected area diffraction pattern studies. In addition, the specific surface area was measured using a Brunauer–Emmett–Teller specific surface area analysis. The hydrogen reduction in different temperature ranges was analyzed using the H₂ temperature-programmed reduction technique. The specific surface area of the ZnFe₂O₄ was 5.66 m²/g, and the specific surface area of the ZnO-ZnFe₂O₄ was 8.20 m²/g at a G/N ratio of 1.5 and at a G/N ratio of 1.7, respectively. The specific surface area of the ZnFe₂O₄ was 6.03 m²/g, and the specific surface area of the ZnO-ZnFe₂O₄ was 11.67 m²/g. The ZnFe₂O₄ and ZnO-ZnFe₂O₄ were found to have the best catalytic effect at 500 °C. In particular, the highest H₂ generation rate of the ZnO-ZnFe₂O₄ (GN = 1.7) at 500 °C was 7745 mL STP min⁻¹ g-cat⁻¹. Moreover, the ZnO-ZnFe₂ O₄ catalyst demonstrated good H₂ selectivity and stability during the process of steam reforming methanol. Therefore, the ZnO-ZnFe₂O₄ catalyst powder exhibited high catalytic activity due to the good dispersibility of the ZnO, which increased the specific surface area of the catalyst. In the future, the catalyst can be applied to the steam reforming of methanol for industrial purposes.