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Iron oxides are widely used as catalysts for photo-Fenton-like processes for dye oxidation. In this study, we report on the synthesis of an α/γ-Fe₂O₃ mixed-phase catalyst with magnetic properties for efficient separation. The catalyst was synthesized using glycine–nitrate precursors. The synthesized α/γ-Fe₂O₃ samples were characterized using scanning electron microscopy, X-ray diffraction spectroscopy (XRD), Raman shift spectroscopy, X-ray photoelectron spectroscopy (XPS), and vibrating sample magnetometer (VSM). The diffraction peaks were indexed with two phases, α-Fe₂O₃ as the main phase (79.6 wt.%) and γ-Fe₂O₃ as the secondary phase (20.4 wt.%), determined using the Rietveld refinement method. The presence of Fe²⁺ was attributed to oxygen vacancies. The mixed-phase α/γ-Fe₂O₃ catalyst exhibited remarkable photo-Fenton-like degradation performance for Rhodamine B (RhB) in neutral pH. The effects of operating parameters, including H₂O₂ concentration, catalyst concentration, and RhB concentration, on the degradation efficiency were investigated. The removal rates of color were 99.2% after 12 min at optimal conditions of photo-Fenton-like oxidation of RhB. The sample exhibited a high saturation magnetization of 28.6 emu/g. Additionally, the α/γ-Fe₂O₃ mixed-phase catalyst showed long-term stability during recycle experiments, with only a 5% decrease in activity.