Two-dimensional (2D) layered oxynitrides are promising candidates as visible-light-driven photocatalysts, but the actual examples are rare because of the difficulty in synthesizing the 2D oxynitrides. Here a phase-pure layered perovskite, RbNdNbON·HO, that belongs to a tetragonal P4/ mmm space group was successfully synthesized by thermal ammonolysis of a mixture of layered RbNdNbO and RbCO, as revealed by synchrotron X-ray diffraction, elemental analyses, and atomic-scale electron microscopy observation. The synthesized RbNdNbON·HO had an absorption edge at around 500 nm and a sufficiently high conduction-band potential to allow for proton reduction. With modification by a platinum cocatalyst, RbNdNbON·HO became photocatalytically active for H evolution in the presence of triethanolamine as an electron donor under visible light (λ > 400 nm).
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