Effect of Nb and Sc Doping on the Phase Transformation of Sol–Gel Processed TiO2 Nanoparticles

Abstract

Nb and Sc doped TiO2 nanoparticles were synthesized via sol–gel technique. Dopant concentration of each element was varied from 0.5 to 1.5 atomic%. The effect of metal ion doping and calcination temperatures on anatase to rutile phase transformation has been investigated. Samples were analyzed by various analytical methods such as X-ray diffraction (XRD), Transmission Electron Microscope (TEM), X-ray Photoelectron Spectroscopy (XPS) and Energy Dispersive X-ray Spectroscopy (EDS). XRD analyses showed that Nb and Sc doped samples calcined at 300 °C and 350 °C, respectively, were crystalline and had an anatase structure. Results showed that anatase was stable up to 700 °C annealing temperature for samples doped with 0.5 atomic% Nb. There was a sharp transition from anatase to rutile phase above 700 °C and complete rutile structure was obtained at 750 °C. However, the transformation from anatase to rutile was not so sharp in samples doped with 1.0 atomic% and 1.5 atomic% Nb. Results indicated that higher concentration of Nb helps to stabilize the anatase phase. For samples doped with 0.5 atomic% Sc, anatase phase is stable up to 650 °C. Transformation from anatase to rutile starts at temperature above 650 °C and 100% rutile phase was obtained at 800 °C while for samples doped with 1.0 atomic% and 1.5 atomic% Sc, the complete transformation from anatase to rutile takes place at an even higher temperature. Results indicate that increasing the calcination time from 0.5 to 2.0 hours at 500 °C does not affect the stability of anatase phase. However, TEM and XRD data showed that the increase in the annealing time leads to an increase in particles size. The rutile to anatase concentration ratio increased with temperature above the phase transformation temperature. The activation energy for the phase transformation from anatase to rutile for doped and undoped samples was also measured. There was a general rise in the activation energy with increasing dopant concentration.