Photoelectrochemical (PEC) water splitting provides an alternative strategy for clean and renewable hydrogen production; however, the practical application is severely limited by the low solar conversion. Herein, a novel and simple strategy has been developed to construct a 3D branched TiO2 photoanode with an ultrathin Al2O3 passivation layer and NiOOH cocatalyst. The structure and properties of the as-obtained photoanodes are explored by X-ray diffraction, Mott–Schottky, electrochemical impedance spectroscopy, and open circuit voltage measurements. The as-obtained B-TiO2/Al2O3/NiOOH ternary heterojunction with a high-quality contact interface exhibits improved light absorption ability, an enhanced photocurrent density of 1.42 mA/cm2 at 1.23 VRHE, high conversion efficiency (0.44% at 0.80 VRHE), and excellent stability compared to pristine TiO2 and alone-Al2O3 or NiOOH decorated TiO2 photoanodes. Therefore, this work could offer a new approach to designing and fabricating high-quality contact interfaces between photoelectrodes and various cocatalysts.

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A layer-by-layer technique has been developed to synthesize FeOOH–Au hybrid nanorods that can be transformed into Fe2O3–Au and Fe3O4–Au hybrid nanorods via controllable annealing process. The homogenous deposition of Au nanoparticles onto the surface of FeOOH nanorods can be attributed to the strong electrostatic attraction between metal ions and polyelectrolyte-modified FeOOH nanorods. The annealing atmosphere controls the phase transformation from FeOOH–Au to Fe3O4–Au and α-Fe2O3–Au. Moreover, the magnetic and optical properties of as-synthesized Fe2O3–Au and Fe3O4–Au hybrid nanorods have been investigated.

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