Abstract Here ZnTiO 3 @TiO 2 heterostructure nanomaterial was prepared through a simple sonochemical strategy using TiO 2 (P25) with zinc nitrate as a precursor and then calcined the obtained sample at 700 °C in 2h for the photocatalytic degradation of Congo red dye solution. XRD result confirms that the diffraction patterns related to the ZnTiO 3 and TiO 2 as heterostructure with high purity. SEM confirms that particles are irregular in shape with high agglomeration and HRTEM reveals that ZnTiO 3 @TiO 2 is highly crystalline with a lattice spacing of 0.37 nm. The calculated band gap of as‐synthesized ZnTiO 3 @TiO 2 heterostructure nanomaterial is found to be 3.07 eV. The photocatalytic degradation of as prepared ZnTiO 3 @TiO 2 heterostructure was investigated for the degradation of Congo red dye by varying the effect of catalyst amount and initial dye concentration. The ZnTiO 3 @TiO 2 heterostructure nanomaterial exhibited 96% degradation efficiency of Congo red in 4h under visible light illumination. Moreover, the photodegradation mechanism of Congo red was studied with various scavengers such as EDTA, IPA, and Benzoquinone. Further, the detection of OH radicals during photocatalytic processes was confirmed by luminescence technique using terephthalic acid (TA) as a test molecule.
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