Synergistic photocatalysis is reported, using the optimal amounts of oxygen vacancies of high‐k materials and nanoarchitecture maneuvering by employing a combinatorial sputtering approach. The highlights include (i) the successful fabrication of samples using combinatorial sputtering; (ii) a systematic investigation of the coupling effect between Y2O3−x and TiO2−x; (iii) elucidating charge carrier transport through current‐voltage (I‐V) and capacitance‐voltage (C‐V) characterizations; and (iv) providing an alternative application for high‐dielectric constant (high‐k) materials in photocatalysis. The simple yet effective composition spread technique rapidly determined that Sample 6 (4 at% Y2O3−x‐96 at% TiO2−x, TiO2−x‐rich on the Y2O3−x–TiO2−x nanorod composite composition spread) exhibited the highest photocatalytic efficiency (i.e., approximately 3.4 times and 1.4 times higher than that of P25 and pure TiO2−x nanorods, respectively). The predominant factor was determined to be electron migration along defective Y2O3−x nanorods to the sample surface. The extracted mobility was discovered to be an order of magnitude greater than that of pure TiO2−x. The photoelectrochemical stability and reusability were also demonstrated.
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