In this study, ZnFe
2O
4 and ZnO-ZnFe
2O
4 catalysts were prepared using the glycine–nitrate process (GNP). The prepared ZnFe
2O
4 and ZnO-ZnFe
2O
4 catalyst powders were characterized using a scanning electron microscope, transmission electron microscope,
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In this study, ZnFe
2O
4 and ZnO-ZnFe
2O
4 catalysts were prepared using the glycine–nitrate process (GNP). The prepared ZnFe
2O
4 and ZnO-ZnFe
2O
4 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 H
2 temperature-programmed reduction technique. The specific surface area of the ZnFe
2O
4 was 5.66 m
2/g, and the specific surface area of the ZnO-ZnFe
2O
4 was 8.20 m
2/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 ZnFe
2O
4 was 6.03 m
2/g, and the specific surface area of the ZnO-ZnFe
2O
4 was 11.67 m
2/g. The ZnFe
2O
4 and ZnO-ZnFe
2O
4 were found to have the best catalytic effect at 500 °C. In particular, the highest H
2 generation rate of the ZnO-ZnFe
2O
4 (GN = 1.7) at 500 °C was 7745 mL STP min
−1 g-cat
−1. Moreover, the ZnO-ZnFe
2 O
4 catalyst demonstrated good H
2 selectivity and stability during the process of steam reforming methanol. Therefore, the ZnO-ZnFe
2O
4 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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