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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.