| Summary: | Compared with traditional hydrothermal synthesis, microwave-assisted synthesis has the advantages of being faster and more energy efficient. In this work, the MoS<sub>2</sub>/BiVO<sub>4</sub> heterojunction photocatalyst was synthesized by the microwave-assisted hydrothermal method within 30 min. The morphology, structure and chemical composition were characterized by X-ray diffraction (XRD), Raman, X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), and high-resolution transmission electron microscopy (HRTEM). The results of characterizations demonstrated that the synthesized MoS<sub>2</sub>/BiVO<sub>4</sub> heterojunction was a spherical structure with dimensions in the nanorange. In addition, the photocatalytic activity of the samples was investigated by degrading tetracycline hydrochloride (TC) under visible light irradiation. Results indicated that the MoS<sub>2</sub>/BiVO<sub>4</sub> heterojunction significantly improved the photocatalytic performance compared with BiVO<sub>4</sub> and MoS<sub>2</sub>, in which the degradation rate of TC (5 mg L<sup>−1</sup>) by compound where the mass ratio of MoS<sub>2</sub>/BiVO<sub>4</sub> was 5 wt% (MB5) was 93.7% in 90 min, which was 2.36 times of BiVO<sub>4</sub>. The active species capture experiments indicated that •OH, •O<sub>2</sub><sup>−</sup> and h<sup>+</sup> active species play a major role in the degradation of TC. The degradation mechanism and pathway of the photocatalysts were proposed through the analysis of the band structure and element valence state. Therefore, microwave technology provided a quick and efficient way to prepare MoS<sub>2</sub>/BiVO<sub>4</sub> heterojunction photocatalytic efficiently.
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