There is an increasing need for environmentally friendly and sustainable energy sources that rely on efficient and abundant electrocatalysts for the oxygen evolution reaction (OER). OER plays a key role in energy conversion and storage applications. Using a vacuum kinetic spray technique operating at room temperature, electrocatalysts based on nano-sized Ni(OH)₂–MoS₂ nanocomposites (NCs) on nickel foam are fabricated from the corresponding micron powders. The Ni(OH)₂–MoS₂ NC modified working electrodes were exploited to investigate the OER at different weight ratios of MoS₂ (25, 50, and 75 wt%). To comprehensively investigate and elucidate the surface state and morphology of the electrode, x-ray diffraction, scanning electron microscopy (SEM), Raman spectroscopy, and x-ray photoelectron spectroscopy (XPS) were assessed. SEM images showed that the micro-sized particles were fragmented into smaller nanoscale particles. XPS spectra revealed the synergy enhancement in the Ni(OH)₂–MoS₂ NCs that resulted in a strong improvement in the OER activity. Ni(OH)₂–MoS₂ hybrid NCs with 75 wt% MoS₂ exhibited the lowest overpotential of 282 mV at 10 mA cm⁻² and a small Tafel slope of 54 mV⋅dec⁻¹. Alongside, the prolonged OER durability at 50 mA cm⁻² is verified for up to 50 h.