Influence of calcination temperatures on the formation of anatase TiO2 nano rods with a polyol-mediated solvothermal method

Abstract

A simple and convenient method has been demonstrated for large-scale synthesis of titanium dioxide (TiO₂). Nano-rod TiO₂ with anatase structure had been prepared by a polyol-mediated solvothermal process of titanium tetra-isopropoxide (TTIP) and ethylene glycol (EG) followed by powder calcination at high temperature. The growth mechanism of the TiO₂ nano-rods was discussed and supported by X-ray diffraction (XRD), Fourier transform infra-red (FT-IR) spectroscopy, Raman spectroscopy, high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and scanning electron microscopy (SEM). Anatase TiO₂ nano-rods (NRs) were synthesized by adjusting the preparation parameters such as precursor concentration, autoclaving temperature and time duration, and calcination temperature. SEM showed TiO₂ NRs of 100 to 250 nm that were produced due to the reaction of 0.7 mL of TTIP with 25 mL EG, autoclaving temperature of 205 °C for a time duration of 12 h, and calcination in air at 600 °C for 1 h. Calcination temperature had a great effect on the production of TiO₂ nano-rods, where well-defined hexagonal NRs were produced at a high calcination temperature of 600 °C for 1 h.