Hatem A. Mahmoud, Aya Ali, Tarek T. Ali, Bahaa M. Abu‐Zied
Abstract This work focused on the synthesis of nickel oxide under varying hydrothermal conditions as a non-precious and efficient catalyst for NaBH 4 hydrolysis to generate hydrogen. The structural, morphological, and textural features of the calcined samples were characterized using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and N 2 -physisorption techniques. XPS analysis confirmed the presence of Ni 2+ and Ni 3+ species, with varying Ni 3+ /Ni 2+ ratios across the samples. The NH-200 samples showed the highest hydrogen generation rate, approximately 1290 at 323 K, attributed to the enhanced redox behavior of Ni 3+ ions. N 2 -adsorption results revealed mesoporous structures with distinct surface areas and pore characteristics. The catalytic performance was evaluated at 35–50 °C, showing enhanced activity with increasing temperature and NaBH 4 concentration (up to 4.5 wt.%). Activation energies were found to be below 59 kJ mol −1 . The catalyst maintained good stability over five consecutive cycles with only a slight performance decline. These findings confirm that NiO is a cost-effective, active, and reusable catalyst for hydrogen generation via NaBH 4 hydrolysis.