Hydrogen storage and release using a solid-state material e.g., sodium borohydride (NaBH₄) may fulfill the requirements for the ‘Hydrogen Economy’. This study reported ZnO-based materials for hydrogen release via the hydrolysis of NaBH₄. Two different metal oxides e.g. CeO₂ and TiO₂ with different weight loading (5 wt.% and 10 wt.%) were used during the synthesis via a simple combustion method. The synthesis procedure offered nanocomposites consisting of ZnO-xTiO₂, and ZnO-xCeO₂ (x = 5 wt.% or 10 wt.%). Diffraction techniques (X-ray (XRD) and electron diffraction (ED)) confirm the phase purity of the material. Diffuse reflectance spectroscopy (DRS) and photoluminescence spectroscopy characterized the optical properties of the materials. The materials displayed a hydrogen generation rate (HGR) of 3000 mL·min⁻¹·g_cat⁻¹. Thermodynamic analysis revealed that ZnO, ZnO-10TiO₂, and ZnO-10CeO₂ catalysts have activation energies of 59.8, 36.8, and 27.5 kJ·mol⁻¹, respectively.