A new mesoporous Zn1-xMxAl2O4 photocatalyst was prepared using the metal-chitosan complexation method with different degrees of Zn2+ cation substitution with cobalt and nickel ions (M = Co2+ and Ni2+). Characterization using X-ray diffraction (XRD), Infrared absorption spectrometry (FTIR), energy dispersion spectroscopy (EDS), diffuse reflectance spectrometry (DRS), scanning electron miscoscopy (SEM), transmission electron miscroscopy (TEM), N2 adsorption- desorption isotherms using the Barrett-Joyner-Halenda (BJH) method, thermogravimetric analysis (TG) and differential thermal analysis (DTA) confirmed the formation of the spinel phase and high purity for all samples. N2 adsorption/desorption and size pore distribution confirmed the high surface area. The photocatalytic activity of Zn1-xMxAl2O4 and the effect of replacing Zn2+ ions with Ni2+ and Co2+ on the degradation of rhodamine B under ultraviolet light were studied in detail. The sample containing 0.1 mol of cobalt had the highest removal rate reaching 83%, favored by surface area and material bandgap (109 m2 g−1 and 2.19 eV, respectively).

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