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Ag3PO4/Ag4P2O7 photocatalysts were successfully synthesized by microwave-hydrothermal method. Tuning the properties of photocatalysts was achieved using different amount of acetic acid (CH3COOH) and sodium hydroxide (NaOH) to adjust pH value of precursor solution (pH = 4, 7, 10 and 12). The crystal structure, morphology and optical property of samples were characterized and explained. The photocatalytic activity of sample was determined by degradation of rhodamine B (RhB) and methyl orange (MO) under a wavelength range of 350–700 nm irradiation. The results demonstrated that the change in shape of particles was not observed whereas the average particle size was decreased with increasing pH value because of the high hydroxide ions (OH−). The sample synthesized in the solution with the pH of 10 exhibited excellent photocatalytic performance and stability because of the highest surface area and the present of Ag4P2O7 on the surface of particles. The highest photodegradation efficiency was 99.34 and 96.12% by degrading RhB and MO, respectively. The enhancement of photocatalytic performance of Ag3PO4/Ag4P2O7 was discussed. The active species trapping experiments showed that the h+ was the main active species to decompose the dye molecules.

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