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• The novel Yb3+/Tm3+ co-doped Ti 3 C 2 /Ag@Ag 3 VO 4 composite was fabricated by in-situ partially reduction-hydrothermal strategy. • The resultant Yb3+/Tm3+ co-doped Ti 3 C 2 /Ag@Ag 3 VO 4 composite exhibited enhanced photo-degradation performance under visible light irradiation. • The synthetic process and the corresponding photocatalytic mechanism was proposed and investigated detailedly. A novel Yb3+/Tm3+ co-doped Ti 3 C 2 /Ag/Ag 3 VO 4 composite with stable and robust photodegradation performance was synthesized by in-situ partially reduction along with hydrothermal strategy. In the composite, block-like Ag 3 VO 4 particles are self-assembled on the surface of 2D Ti 3 C 2 MXene accompanied by partial reduction of Ag+ to Ag0. Photodegradation results showed that the resulting Yb3+/Tm3+ co-doped Ti 3 C 2 /Ag/Ag 3 VO 4 composite with optimal Yb/Tm proportion (Y/T:0.3/0.005) presented a boosting photocatalytic performance for degradation of tetracycline (TC) and organic dyes under visible light irradiation. The removal efficiency was 97% for TC in 20 min, 96% for rhodamine B in 25 min, and 99% for methylene blue in 20 min, which was higher than that of Ag/Ag 3 VO 4 composite. As manifested by photoelectrochemical measurements, the enhanced photocatalytic performance of the Y/T:0.3/0.005 composite was attributed to the improved light absorption and excellent charge separation induced by the formation of intermediate energy states after co-doping Yb3+/Tm3+ ions. Meanwhile, the photocatalytic mechanism of the photocatalyst was also investigated through electron spin resonance (ESR) spectra and trapping experiments, which verified that the active species of h+ and ·O 2 − play the important role for photodegradation of tetracyline and organic dyes. [ABSTRACT FROM AUTHOR]