SOL-GEL SYNTHESIS AND ADVANCED CHARACTERISATION OF TITANIUM DIOXIDE NANOPARTICLES

Wisdom Chukwuemeke   Ulakpa; Oluwatosin Sarafa  Azeez; Moses Aderemi    Olutoye

doi:10.4314/njt.v44i3.4

Authors

W. C. Ulakpa Department of Chemical Engineering, Faculty of Engineering, Federal University of Technology, Minna, Nigeria https://orcid.org/0000-0002-3128-5956
O. S. Azeez Department of Chemical Engineering, Faculty of Engineering, Federal University of Technology, Minna, Nigeria https://orcid.org/0000-0002-2628-3227
M. A. Olutoye Department of Chemical Engineering, Faculty of Engineering, Federal University of Technology, Minna, Nigeria https://orcid.org/0000-0003-2893-1475

DOI:

https://doi.org/10.4314/njt.v44i3.4

Keywords:

Sol-gel Synthesis, Calcination, Nano-particles, Titanium dioxide, Anatase, Characterization

Abstract

The sol-gel method was used in this study to synthesis Titanium Dioxide (TiO2) Nanoparticles (NPs) using Titanium (iv) isopropoxide as precursor material. Thereafter, the resultant xerogel was calcined at 400 ^OC. The synthesized nanoparticles were dried at 100ºC for 2 hours and calcined at 400ºC for 3 hours. The particles were characterized by Thermogravimetric analysis/differential scanning calorimetry (TGA/DSC), high-resolution transmission electron microscopy (HRTEM), Brunauer-Emmett-Teller (BET/BJH) analysis, X-ray diffraction (XRD), X-ray fluorescence (XRF), Field Emission Scanning Electron Microscopy (FESEM), Fourier-transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). The nanoparticles revealed an anatase phase when heated to 400˚C, according to the X-ray diffraction (XRD) examination. Further analysis revealed a crystallite size of 11.71 nm and an average particle size of 24.48 nm for the nanoparticles. The investigation additionally showed that the nanoparticles exhibited 11.71 nm crystallites with particles sized of 24.48 nm on average. Spherical particles with a diameter of at least 50 nm were visible in TEM examinations. In agreement with TEM results, XRD data verified the particles' excellent purity and crystallinity. The BET/BJH result shows a mean pore width of 3.685 nm which indicate mesoporous structure, pore volume of 0.04367 cm3g, and surface area of 23.701 m²/g. The Ti 2p orbital was found to exist in the oxidation states of +4 by X-ray photoelectron spectroscopy. This work focuses on the production of TiO₂ nanoparticles using a simple sol-gel synthesis technique and their thorough characterisation. The objective of this research is create titanium dioxide nanoparticles with better stability, reactivity, and performance than conventional methods and to promote the development of advanced materials with particular properties for use in photocatalysis and biodiesel generation, among other fields.

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