Heterostructures constructed in various dimensions have received considerable attention as promising platforms for improving activity of photocatalytic materials. Herein, two-dimensional (2D) high crystalline g-C3N4 (HCCN) nanosheets were loaded onto the surface of three-dimensional (3D) yolk-shell ZnFe2O4 (ZFO) to construct 2D/3D HCCN/ZFO heterojunction by a simple two-step process consisting of a solvothermal method and a calcination process. It is found that the formation of heterojunction can effectively enhance photo-absorption and separation efficiency of carriers. In contrast to pure HCCN and ZFO, the tetracycline (TC, 30 mg/L) degradation rate of optimal 20% HCCN/ZFO heterojunction can be reached 85%, and degradation rate constant is 0.0133 min−1, which is 3.8 and 4.9 times higher than HCCN (0.0035 min−1) and ZFO (0.0027 min−1), respectively. Besides, the reasonable mechanism of photocatalytic degradation of TC and possible intermediates products were discussed based on the results of capture experiments, electron spin resonance (ESR) and liquid chromatography-mass spectrometry (LC-MS).

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