We report the annealing effects on the structural, optical, and electrical properties of 〈111〉-single-oriented Cu2O films electrodeposited on Au(111)/Si(100) substrates from an aqueous solution (pH = 12.5) containing copper acetate and lactic acid. Annealing at 250–400 °C was performed in air and in an Ar atmosphere, and characterization was performed using an X-ray diffractometer, a field-emission scanning electron microscope, an X-ray photoelectron spectroscope, and photoluminescence and Hall effect measurements. It was found that annealing affects the Cu2O/Au interface by thermal diffusion of Si as well as the crystallinity of Cu2O. Photoelectric properties were also evaluated by two different methods of measuring internal photoelectric current and photoelectrochemical current under light illumination. Compared with the as-deposited Cu2O films, the Cu2O films annealed at 300 °C in Ar exhibited optimal photoelectric performances resulting from a 25 times increase in carrier mobility and a decrease in native defects.
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