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Photocatalytic hydrogen production is a sustainable method to alleviate the energy crisis. Herein, the Co2P/TiO2 Z‐scheme junction photocatalysts without noble metal are synthesized by a simple hydrothermal method. Compared to pure TiO2 simple, the Co2P/TiO2 Z‐scheme junction photocatalysts exhibit much more excellent photocatalytic H2‐evolution activity, which suggests the Z‐scheme junction has a positive influence on the photocatalytic hydrogen production. Particularly, the optimal 3 wt% Co2P/TiO2 displays the most outstanding photocatalytic activity with the hydrogen evolution rate of 409.5 μmol h−1 g−1, which exceeds that of pure TiO2 by almost 17 times (23.6 μmol h−1 g−1). The function of Z‐scheme junction in Co2P/TiO2 hybrid that enhances the separation of electron–hole pairs is confirmed by the photoluminescence spectra, electrochemical impedance spectroscopy, and transient photocurrent responses. It is also suggested in these results that the Co2P is a cocatalyst in Co2P/TiO2 system. And, the process of electron transfer is investigated by the Kelvin probe instrument. It is clearly demonstrated that the Z‐scheme junction plays a significant role in the effective charge separations of holes and electrons. Herein, a new method of synthesizing TiO2‐based photocatalysts with high photocatalytic performance is offered.

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