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1 Supporting Information for Effect of Ti 3+ Ions and Conduction Band Electrons on Photocatalytic and Photoelectrochemical Activity of Rutile Titania for Water Oxidation Fumiaki Amano a *, Masashi Nakata a, Akira Yamamoto b, and Tsunehiro Tanaka b a Department of Chemical and Environmental Engineering, Graduate School of Environmental Engineering, The University of Kitakyushu, 1-1 Hibikino, Wakamatsu-ku, Kitakyushu , Japan. b Department of Molecular Engineering, Graduate School of Engineering, Kyoto University, Kyoto Daigaku Katsura, Nishikyo-ku, Kyoto , Japan. S1
2 Table S1. Physical properties and photocatalytic activities of commercial TiO2 particles. sample supplier XR a (wt%) SSA b (m 2 g 1 ) Ag + on TiO2 c (μmol g 1 ) r(o2) d (μmol h 1 ) rutile TiO2 (R-Kojundo) P25 FP-6 anatase TiO2 Kojundo Chemical Laboratory (Sakado, Japan) Nippon Aerosil (Yokkaichi, Japan) Showa Titanium (Toyama, Japan) Kanto Chemical (Tokyo, Japan) a) Weight fraction of rutile in the anatase-rutile mixture, b) BET specific surface area, c) the amount of Ag + ion adsorbed on TiO2 in dark, d) rate of photocatalytic O2 evolution by water oxidation over 5-mg TiO2 in the presence of AgNO3, and e) Degussa (Evonik) P25. S2
3 Solution exchange 1 1st run 2nd run O 2 evolution / mol Irradiation / min Figure S1. Time course for the photocatalytic O2 evolution by water oxidation in the presence of sacrificial AgNO3 over R-Kojundo. The solution was changed after irradiation for 12 min due to the consumption of Ag + ions (45 µmol). The Ag + ions are reduced to silver particles, which are deposited on TiO2 surface. The r(o2) was not affected by the decrease of the Ag + concentration and the deposition of silver particles. S3
4 Figure S2. TEM images of R-Kojundo (a) before and (b) after photocatalytic O2 evolution for 12 min. The amount of photodeposited Ag, which was measured by ICP-OES after dissolving with HNO3, was consistent with the stoichiometric amount calculated from the evolved O2 (4 electrons are required for the evolution of one molecule of O2). S4
5 a Normalized intensity b c d e / degree Figure S3. XRD patterns of (a) R-Kojundo, (b) R5, (c) R7, (d) R9, and (e) R11: () rutile TiO2, ( ) anatase TiO2, and ( ) NiO mixed as an internal standard. The patterns have been translated in the Y-axis for clarity. S5
6 Normalized intensity a b c / degree Figure S4. XRD patterns of (a) R9, (b) R9-H5, and (c) R9-H7: () rutile TiO2 and ( ) NiO mixed as an internal standard. The patterns have been translated in the Y-axis for clarity. S6
7 Normalized intensity a b c / degree Figure S5. XRD patterns of (a) R11, (b) R11-H5, and (c) R11-H7: () rutile TiO2 and ( ) NiO mixed as an internal standard. The patterns have been translated in the Y-axis for clarity. S7
8 Rate of O 2 evolution / mol h H 2 reduction temperature / C Figure S6. Effect of temperature of H2 treatment on the rate of photocatalytic O2 evolution of R11. S8
9 Figure S7. FE-SEM images of (a) R-Kojundo, (b) R11, and (c) R11-H7. S9
10 1 8 R7 R7-H5 R7-H7 1-%R Wavelength / nm 8 R9 R9-H5 R9-H7 1-%R Wavelength / nm Figure S8. Diffuse reflectance UV-Vis-NIR spectra of TiO2: (a) R7, (b) R7-H5, (c) R7-H7, (d) R9, (e) R9-H5, and (f) R9-H7. S1
11 Figure S9. Pictures of thermally oxidized TiO2 films on titanium sheet. S11
12 Intensity / arb.unit Ti9 Ti9-H4 Ti9-H / degree Figure S1. XRD patterns of (a) Ti9, (b) Ti9-H5, and (c) Ti9-H7: () rutile TiO2. The patterns have been translated in the Y-axis for clarity. S12
13 1 1 - %R Ti9 H3 H6 H55 H5 H45 H Wavelength / nm Figure S11. Diffuse reflectance UV-Vis-NIR spectra of thermally oxidized TiO2 films on titanium sheet. S13
14 C -2 / cm 4 F -2 5x1 14 4x1 14 3x1 14 2x1 14 Ti9 Ti9-H3 Ti9-H4 Ti9-H45 Ti9-H5 Ti9-H55 Ti9-H6 1x1 14 C -2 / cm 4 F -2 8x1 11 6x1 11 4x Potential / V vs. Ag-AgCl Ti9-H45 Ti9-H5 Ti9-H55 Ti9-H6 2x Potential / V vs. Ag-AgCl Figure S12. Mott Schottky plots of thermally oxidized TiO2 films on titanium sheet in.1 mol L 1 H2SO4 (ph = 1). S14
15 Current density / ma cm -2 Current density / ma cm under irradiation H6 H55 H45 H5 H4 Ti9 H Potential / V vs. Ag-AgCl.4 in dark H6_dark H55_dark.3 H5_dark H45_dark H4_dark H3_dark.2 Ti9_dark Potential / V vs. Ag-AgCl Figure S13. Current density-anodic potential curves of thermally oxidized TiO2 films in.1 mol L 1 H2SO4 (ph = 1) under photoirradiation and in dark. S15
16 O 2 evolution / mmol H6 H45 H55 H Irradiation time / min H4 Ti9 H3 Figure S14. Rate of photocatalytic O2 evolution by water oxidation in the presence of sacrificial AgNO3 over thermally oxidized TiO2 films on titanium sheet. S16
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