| Summary: | Targeting heterostructures with modulated electronic structures and efficient charge carrier separation and mobility is an effective strategy to improve photocatalytic performance. In this study, we report the synthesis of 2D/3D hybrid heterostructures comprising P-doped graphitic carbon nitride (g-C<sub>3</sub>N<sub>4</sub>) nanosheets (ca. 50–60 nm in lateral size) and small-sized Ni<sub>2</sub>P nanoparticles (ca. 10–12 nm in diameter) and demonstrate their prominent activity in the photocatalytic reduction of Cr(VI). Utilizing a combination of spectroscopic and electrochemical characterization techniques, we unveil the reasons behind the distinct photochemical performance of these materials. We show that Ni<sub>2</sub>P modification and P doping of the g-C<sub>3</sub>N<sub>4</sub> effectively improve the charge-carrier transportation and spatial separation through the interface of Ni<sub>2</sub>P/P-doped g-C<sub>3</sub>N<sub>4</sub> junctions. As a result, the catalyst containing 15 wt.% Ni<sub>2</sub>P exhibits superior photocatalytic activity in the detoxification of Cr(VI)-contaminated effluents under UV-visible light illumination, presenting an apparent quantum yield (QY) of 12.5% at 410 nm, notably without the use of sacrificial additives. This study marks a forward step in understanding and fabricating cost-effective photocatalysts for photochemical applications.
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