<p>In this study, NiWO₄ and Pd-doped NiWO₄ (Pd_0.05Ni_0.95WO₄) nanocrystals were synthesized via a sol-gel hydrothermal method using polyvinyl alcohol as a surfactant. The resulting nanoparticles were characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and energy-dispersive spectroscopy (EDS). XRD analysis confirmed the monoclinic crystal phase, with a significant reduction in crystallite size from 60 nm for NiWO₄ to 29 nm upon Pd incorporation. SEM images revealed agglomerated particles with a distinct needle-like morphology, while XPS verified the successful incorporation of Pd and the presence of mixed W⁶⁺ and W⁵⁺ oxidation states in Pd_0.05Ni_0.95WO₄. The catalytic performance of NiWO₄ and Pd_0.05Ni_0.95WO₄ as cathodes for the hydrogen evolution reaction (HER) in alkaline media was evaluated. The Pd_0.05Ni_0.95WO₄ /NF electrode exhibited superior electrocatalytic activity, achieving a cathodic current density of 237.1 mA cm⁻² at −1.5 V, compared to 147.2 mA cm⁻² for NiWO₄/NF. Additionally, the Pd-doped electrode demonstrated a significantly lower overpotential of 223.2 mV at a current density of 20 mA cm⁻² (η₂₀), compared to 323.2 mV for NiWO₄/NF. At −1.25 V, Pd_0.05Ni_0.95WO₄/NF exhibited a reduced charge transfer resistance (R_ct) of 2.05 Ω cm², significantly lower than the 3.8 Ω cm² observed for NiWO₄/NF, indicating enhanced charge transfer kinetics.</p> Graphical Abstract <p></p>