Dion–Jacobson type layered perovskite niobium oxides KCa2Nb3O10 and KSr2Nb3O10 were prepared via molten salt method, and the potassium cations were exchanged by protons using nitric acid. Different degrees of proton exchange were adjusted, and the dependence of photocatalytic activity for hydrogen evolution on proton exchange was investigated. Moreover, proton exchange leads to different amounts of water incorporated into the interlayer spaces, also influencing photocatalytic performance significantly. Decoupling water intercalation and proton exchange, the photocatalytic activity of proton exchanged KCa2Nb3O10 and KSr2Nb3O10 can be revealed and tailored.
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