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TiO  x  N  y  /TiO 2 was synthesized by nitriding of TiO 2 in NH 3 gas. TiO  x  N  y  /TiO 2 generated hydrogen from methanol aqueous solution under visible-light irradiation. It was revealed by N K-edge XANES and N 1s XPS measurements that the N species contributing to visible-light responsiveness was the O-Ti-N species. The structure of TiO  x  N  y  /TiO 2 showing the photocatalytic activity was a double shell type with thin layers of TiO  x  N  y  that covers the TiO 2 core. Although N content on the surface decreased during the photocatalytic reaction, N was supplied from the deeper side to keep the TiO  x  N  y  phase at the surface and the activity as well.

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TiOxNy/TiO2 Photocatalyst for Hydrogen Evolution under Visible-Light Irradiation. I: Characterization of N in TiOxNy/TiO2 Photocatalyst