Wide band gap semiconductor niobate photocatalysts with Dion-Jacobson layered perovskite structure were nitrogen-doped via simple gas–solid reaction to extend their absorption into the visible light range. Nitrogen doping was performed using ammonia as precursor, resulting in decreased band gaps of doped AB2Nb3O10 compounds (A = Cs, Rb, K; B = Ca, Sr) down to 2.5 eV. The resulting materials were investigated concerning their chemical and electronic structures. Nitrogen-doped AB2Nb3O10 crystals showed a clear red shift in absorption. Photocatalytic performance tests for the doped materials evaluated the capability of H2 production under simulated solar irradiation. The addition of carbonates to the gas–solid reaction turned out to be advantageous for the reduction of defects and the preservation of photocatalytic activity of nitrogen-doped layered niobates AB2Nb3O10.
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