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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.

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