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The photocatalytic hydrogen evolution reaction is one of the most promising approaches to utilize solar energy and produce hydrogen as an alternative energy source to traditional fossil fuels. In this work, we focused on further exploring the cocatalyst potential of the transition metal nickel and prepared nickel oxide/carbon nitride (NiO/CN_x) heterojunctions through thermal polymerization as well as plasma-enhanced atomic layer deposition (PEALD). The optimal NiO loading thickness on the surface of the CN_x was found to be 6.5 nm, prepared from 65 cycles of ALD. This NiO(65)/CN_x had a photocatalytic hydrogen evolution rate of 3.9 μmol h^–1 in a 2 mg mL^–1 aqueous photocatalyst solution (195 μmol h^–1 g^–1), corresponding to an AQY of 3.1% and exhibiting 54% of the activity of 3 wt % Pt/CN_x under 405 nm light illumination with a sacrificial reagent. A 3 wt % Ni/CN_x prepared through a photodeposition process …