| Summary: | In the present work, we have reported a facile and large-scale synthesis of TiO<sub>2</sub> nanoparticles (NPs) through urea-assisted thermal decomposition of titanium oxysulphate. We have successfully synthesized TiO<sub>2</sub> NPs by using this effective route with different weight ratios of titanium oxysulphate: urea. The structures and properties of TiO<sub>2</sub> NPs were confirmed by scanning electron microscope) (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), fourier transform infrared spectroscopy (FT-IR), ultra violet–visible spectroscopy (UV-vis), and photoluminescence (Pl) techniques. XRD demonstrated that TiO<sub>2</sub> NPs holds of anatase crystal phase with crystallizing size 14–19 nm even after heating at 600 °C. TGA, SEM, and TEM images reveal urea’s role, which controls the size, morphology, and aggregation of TiO<sub>2</sub> NPs during the thermal decomposition. These TiO<sub>2</sub> NPs were employed for photodegradation of Methyl Orange (MO) in the presence of ultraviolet (UV) radiation. An interesting find was that the TiO<sub>2</sub> NPs exhibited better photocatalytic activity and excellent recycling stability over several photodegradation cycles. Furthermore, the present method has a great perspective to be used as an efficient method for large-scale synthesis of TiO<sub>2</sub> NPs.
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