Ultrasonic-assisted pH Swing Method for the Synthesis of Highly Efficient TiO2 Nano-size Photocatalysts

A new route for the preparation of nanocrystalline TiO₂ particles based on the pH swing method assisted by ultrasonic irradiation in the presence of a surfactant (Pluronic P-123) has been successfully achieved. The prepared TiO₂ catalysts were calcined from 400 to 800 °C and characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transformed infra-red spectroscopy (FTIR), gas adsorption measurements (BET) and thermogravimetirc measurements (TAG/DTA) analyses. Characterization results revealed that the enhancement in the particle size of TiO₂ by the pH swing method could be controlled by combining the pH swing with ultrasonic irradiation. Increasing the calcination temperatures led to an increase in both the particle and pore size, whereas the surface area and pore volume gradually decreased. A synergistic effect was observed in the combined process of pH swing with ultrasonication, yielding small TiO₂ particles as well as high surface area, pore volume, pore diameter, and crystalline anatase phase. The activity of the catalysts was investigated for the oxidation of 4-chlorophenol (4-CP). TiO₂ prepared with 15 times pH swing and calcined at 700 °C was found to show the highest rate for the oxidative degradation of 4-CP when compared to the TiO₂ sample prepared with just 1 time pH swing and to the commercial P-25 TiO₂ Degussa photocatalyst. Thus, a novel approach in controlling the various physico-chemical parameters of TiO₂ nanoparticles was developed.