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Photocatalytic degradation has been suggested to be a cheap and efficient way to dispose of organic pollutants, such as dyes. Therefore, our research team strives to produce nanophotocatalysts in a simple and inexpensive way. In this work, the Pechini sol–gel technique was employed for the facile synthesis of Mn0.5Zn0.5Fe2O4/Fe2O3 and Fe0.5Mn0.5Co2O4/Fe2O3 as mixed metal oxide nanoparticles for the efficient photocatalytic degradation of Rhodamine B and Congo Red dyes. XRD, FT-IR, a N2 adsorption/desorption analyzer, EDS, FE-SEM, and an UV–Vis diffuse reflectance spectrophotometer were used to characterize the produced samples. The XRD patterns revealed that the average crystallite size of the Fe0.5Mn0.5Co2O4/Fe2O3 and Mn0.5Zn0.5Fe2O4/Fe2O3 samples is 90.25 and 80.62 nm, respectively. The FE-SEM images revealed that the Fe0.5Mn0.5Co2O4/Fe2O3 sample consists of cubic and irregular shapes with an average diameter of 1.71 µm. Additionally, the Mn0.5Zn0.5Fe2O4/Fe2O3 sample consists of spherical shapes with an average diameter of 0.26 µm. The energy gaps of the Fe0.5Mn0.5Co2O4/Fe2O3 and Mn0.5Zn0.5Fe2O4/Fe2O3 samples are 3.50 and 4.3 eV and 3.52 and 4.20 eV, respectively. In the presence of hydrogen peroxide, the complete degradation of 100 mL of 20 mg/L of Rhodamine B and Congo Red dyes occurred at pH = 8 and 3, respectively, within 50 min, using 0.1 g of the synthesized samples.

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