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The precise modification of redox species on the inner and outer surfaces of hollow nanostructures is relevant in catalysis, surface science, and nanotechnology, but has proven difficult to achieve. Herein, we develop a facile approach to specifically fabricate Pt and Co 3 O 4  nanoparticles (NPs) onto the interior and exterior surface of hollow carbon nitride spheres (HCNS), respectively, to promote the surface redox functions of the polymer semiconductors. The photocatalytic water splitting activities of HCNS with spatially separated oxidation and reduction centers at their nanodomains were enhanced. The origin of the enhanced activity was attributed to the spatially separated reactive sites for the evolution of H 2  and O 2  and also to the unidirectional migration of the electron and hole on the Janus surfaces, thereby preventing the unwanted reverse reaction of water splitting and decreasing charge recombination.

Precise Formation of a Hollow Carbon Nitride Structure with a Janus Surface To Promote Water Splitting by Photoredox Catalysis