This work investigates the potential of ZrO2/MoO3 nanocomposites as catalysts for hydrogen production through NaBH4 methanolysis. The samples were prepared by controlled thermal calcination and characterized using various techniques like XRD, FTIR, Raman, SEM, and surface area BET analysis. Rietveld refinements verified the presence of the ZrO2 monoclinic phase with the space group P21/c in all samples and a second orthorhombic MoO3 phase with the space group Pnma. The average crystal size decreased from 44 to 40 nm. FTIR and Raman spectroscopy confirmed the successful preparation of ZrO2/MoO3 nanocomposites. SEM analysis showed ZrO2 particles and MoO3 nanoparticles adhered to the ZrO2 surface, potentially creating a rougher texture. The results confirmed the formation of ZrO2/MoO3 nanocomposites with increasing MoO3 content, leading to an increased surface area of 19–23 m2/g. The catalytic performance evaluation revealed that the sample containing 30 % MoO3 (ZM3) exhibited the highest hydrogen generation rate of 18,451 mL/g. min at 30 °C. The calculated activation energy for ZM3 was 18.78 kJ/mol, suggesting efficient hydrogen generation at moderate temperatures.