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Herein, Zn3In2S6 photocatalyst with (110) exposed facet was prepared by low temperature solvothermal method. On this basis, a highly efficient binary Zn3In2S6/g-C3N4 was obtained by low temperature solvothermal method and applied to the degradation of tetracycline (TC). The samples of the preparation were characterized by X-ray diffraction, scanning electron microscope, transmission electron microscope, UV–vis diffuse reflection spectroscopy, and photoluminescence spectroscopy. Furthermore, the degradation performance of photocatalysts on TC was investigated under different experimental conditions. Finally, the mechanism of Zn3In2S6/g-C3N4 composite material degrading TC is discussed. The results show that Zn3In2S6 and Zn3In2S6/g-C3N4 photocatalysts with excellent performance could be successfully prepared at lower temperature. The Zn3In2S6/g-C3N4 heterojunction photocatalyst could significantly improve the photocatalytic activity compared with g-C3N4. After 150 min of illumination, the efficiency of 80%Zn3In2S6/g-C3N4 to degrade TC was 1.35 times that of g-C3N4. The improvement of photocatalytic activity was due to the formation of Zn3In2S6/g-C3N4 heterojunction, which promoted the transfer of photogenerated electron–holes. The cycle experiment test confirmed that Zn3In2S6/g-C3N4 composite material had excellent stability. The free radical capture experiment showed that ·O2− was the primary active material. This study provides a new strategy for the preparation of photocatalysts with excellent performance at low temperature.

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