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TiO2 is a promising photocatalyst due to its high thermodynamic stability and non-toxicity. However, its applications have been still limited because of the high recombination rate of electron–hole pairs. Herein, we show that by combining heterojunction construction and electronic structure regulation, the electron–hole pairs in TiO2 can be effectively separated for enhanced photocatalytic hydrogen evolution. The optimized Cu7S4 nanosheet decorated TiO2 achieves much enhanced H2 evolution rate (11.5 mmol·g−1·h−1), which is 13.8 and 4.2 times of that of TiO2 and Cu7S4/TiO2, respectively. The results of photoluminescence spectroscopy, transient photocurrent spectra, ultraviolet–visible diffuse reflectance spectra, and electrochemical impedance spectroscopy collectively demonstrate that the enhanced photocatalytic performance of Air-Cu7S4/TiO2 is attributed to the effective separation of charge carriers and widened photoresponse range. The electron paramagnetic resonance and X-ray photoelectron spectroscopy results indicate that the increase of Cu2+ in the Cu7S4 nanosheet after calcination can promote the charge transfer. This work provides an effective method to improve the electron migration rate and charge separation of TiO2, which holds great significance for being extended to other material systems and beyond.
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