| Summary: | AgI/MFeO<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub> (M = Y, Gd, La) nano sheet–sphere–sheet photocatalysts were synthesized by a simple ultrasound-assisted hydrothermal approach. We characterized the microstructure, surface morphology, and optical absorption capacity of the obtained samples. According to the characterization results, AgI/MFeO<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub> (M = Y, Gd, La) nano sheet–sphere–sheet photocatalysts were successfully obtained. MFeO<sub>3</sub> nanospheres and AgI nanosheets were dispersed evenly on the surface of g-C<sub>3</sub>N<sub>4</sub> nanosheets. AgI/MFeO<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub> showed remarkable photocatalytic. Especially, 95% of NOF was photodegradated over AgI/LaFeO<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub> within 3 h and the higher photocatalytic performance still remained after six cycles. Additionally, The N<sub>2</sub> adsorption–desorption isotherms of AgI/MFeO3/g-C<sub>3</sub>N<sub>4</sub> showed that AgI/LaFeO<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub> possessed the highest specific surface area (79.32 m<sup>2</sup>/g). The result of scavenging experiment revealed that ·O<sub>2</sub><sup>−</sup>, h<sup>+</sup>, and ·OH were the main roles in the photodegradation process. Benefitting from the nice energy band matching, MFeO<sub>3</sub> acted as the center of photogenerated electrons migration and separation provided more direct electron channels. This work proposes an effective approach for the design and configuration of dual Z-scheme photocatalysts to accomplish the removal of organic contaminants based on g-C<sub>3</sub>N<sub>4</sub>.
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