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The corresponding time course is shown inFigure S4(see theSupporting Information). Reproducibility tests using different batches of Pt/ZrO2/TaON showed that the obtained AQY slightly varied from batch to batch but remained within 10%. Because the ratio of H2to O2evolution was sometimes slightly higher than that expected from the stoichiometry, we calculated the AQYs on the basis of the rates of O2evolution derived from the two-step water splitting cycle.
In this case, the NaI concentration was 1.0 mM (15 mg in 100 mL of solution).
Kudo, A.“Nano-structured Photocatalysts for Solar Water Splitting”,ICACC Symposium 74th International Symposium on Nanostructured Materials and Nanocomposites: Development and Applications, Dayton Beach, FL, USA, January 28, 2010.
As shown inFigure S5, no O2evolution was observed in the initial stage of the reaction, due primarily to the detection limit of our gas chromatograph. The AQYs calculated from the initial H2evolution rate and the O2evolution rate were ca. 1 and 0.2%, respectively.
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Porous ZrO2/TaON and TaON electrodes were prepared by pasting viscous slurry onto conducting glass according to a previously described method.(61)A mixture of 50 mg of as-prepared ZrO2/TaON (or TaON) powder (particle size 300−500 nm), 10 μL of acetylacetone (Kanto Chemicals), 10 μL of TritonX (Aldrich), 10 μL of poly(ethylene glycol) 300 (Kanto Chemicals), and 250 μL of distilled water was ground in an agate mortar to prepare the viscous slurry. The slurry was then pasted onto fluorine-doped tin oxide (FTO) glass slides (12 Ω sq−1, transparency 80%, thickness 1 mm; Asahi Glass, Japan) to prepare a 1 × 4 cm2electrode, and the sample was calcined in a nitrogen gas flow at 673 K for 1 h. Thermogravimetric and differential thermal analysis revealed that almost no carbon species, derived from additives in the preparation, are persistent in the as-prepared electrode.
Measurements were performed using a conventional Pyrex electrochemical cell with a platinum wire as a counter electrode and an Ag/AgCl reference electrode under potentiostat control (HSV-100, Hokuto Denko, Japan). Current−voltage curves were measured in an aqueous sodium sulfate solution (Na2SO4, 0.1 M, 100 mL) as a supporting electrolyte. The electrolyte solution was purged with nitrogen prior to the measurements and was maintained at room temperature by a flow of cooling water during the measurements. A 300 W xenon lamp fitted with a cutoff filter was used as a visible light irradiation source. The effective irradiation area was 1 × 3.5 cm2.
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