Pure and Iron doped TiO2 nanoparticles were synthesized using the sol-gel method. These materials were characterized by X-ray diffractometer (XRD), high-resolution transmission electron microscope (HR-TEM), scanning electron microscope (SEM), Energy dispersive X-ray (EDX), UV–Vis diffuse reflectance spectroscopy (DRS), Fourier-transform infrared (FTIR), Raman and fluorescence spectrometer. XRD analysis revealed that all the samples were a single phase with anatase nanocrystallite structures. The crystallite size of titania reduced from 9.64 nm to 7 nm with Fe doping. The HRTEM images of the TiO2 and 3% Fe doped TiO2 have revealed that all the particles have a spherical shape with an average particle size of 10 nm and 8 nm respectively. The characteristic peak at 482 cm−1 of the Ti O bond stretching vibrations can be evidently observed from FTIR analysis. The Raman blue shift was found in the Fe doped TiO2 samples. Fe-doped TiO2 nanoparticles showed a significant red-shift in band edge as compared with pure TiO2 nanoparticles. The redshift of band gap was detected in Fe doped TiO2 nanoparticles. The photoluminescence (PL) emission intensity of Fe doped TiO2 nanoparticles decreases with an increase in Fe doping concentration. The photocatalytic efficiencies of the Fe-doped TiO2 nanoparticles have shown a strong photocatalytic activity (PCA) response. At constant irradiation time, the Fe-doped titania nanoparticles display more catalytic activity compared to undoped TiO2. The photodegradation efficiencies typically decline with an increase in the concentration of Fe+3 doping for the decolorization of methylene blue (MB) under visible light irradiation.