This research reports a simple, innovative, and low-cost doping method of TiO2 nanoparticles presenting the effects of calcination and the weight ratio of TiO2:FeCl3 (1:0.33–1:4.5). The photocatalytic activity of the nanomaterials was investigated by decolorizing Rhodamine B (RhB) dye in an aqueous solution. The main results showed that there is anatase-to-rutile transformation after the calcination process. The Fe-doped process modified the TiO2 spectrum and showed a connection in the Ti–O–Fe vibration. The particle size is within the nanometer range, between 20–51 nm, except for calcined TiO2. The inclusion of Fe in TiO2 decreased the band gap energy from 3.16 (reference) up to 2.06 eV (1:3). Additionally, after the calcination, there was a decrease in this value from 3.03 eV (reference) up to 1.95 eV (1:1.6). The TiO2, with a ratio of (1:1.6), showed the highest activity in the photocatalytic degradation of RhB with an efficiency of 93.8% after 3 h of irradiation.
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