| Summary: | The synthesis of orthoferrites of the type La<sub>1−x</sub>Ce<sub>x</sub>FeO<sub>3+x/2</sub>, x = 0.00, 0.01, 0.03, 0.05, and 0.07, by applying a simple and effective mechanochemical transformation from the constituent oxides is presented. Physicochemical methods such as powder X-ray diffraction (XRD), transmission electron microscopy (TEM), UV–Vis spectroscopy, and Brunauer–Emmett–Teller (BET) adsorption were applied to gain information about the effect of Ce<sup>4+</sup> content on the structural, textural, and optical properties of the samples. The catalytic activity of the samples for water decontamination was determined in a photo-Fenton-like activation of persulfate for removal of tetracycline hydrochloride as model pollutant. The presence of persulfate, PDS, considerably increased the removal efficiency under visible light illumination.
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