Abstract

Abstract A visible-light-responsive nitrogen-doped solid-acid photocatalyst HNb3O8-N is investigated via solid-state high-resolution NMR spectroscopy. The 1H magic-angle-spinning (MAS) spectrum observed under an ultrahigh field of 21.8 T is found drastically different from that of the precursor catalyst HNb3O8. The 1H signals of HNb3O8-N are assigned with the help of 1H–93Nb and 1H–15N two-dimensional heteronuclear correlation (HETCOR) spectroscopy. It is clarified that H3O+ ions contained in HNb3O8 change into H2O and H+, the latter of which protonates NbO6 octrahedra. Deduced from the 1H chemical shift for the nitrogen-adjacent protons, three microstructure models for HNb3O8-N, involving the proton-exchange model, are proposed.

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