Synthesis and Characterization of Titanium Oxide Nanomaterials Using Sol-Gel Method

Abstract

This paper reports the effect of temperature on the properties of TiO_2 nanomaterials, synthesis and characterization. TiO2 powders were synthesized by sol-gel method using TiCl4 solution added in deionized water in ice bath under fume hood followed by the addition of ethanol with vigorous stirring for 30 min at room temperature. The gel solution was obtained and then got dried using oven at 200oC for 4 hours. Then, the dried gel was calcinated at 250oC, 400oC and 600oC using furnace for 4 hours each. The synthesized TiO2 nanomaterials were characterized by XRD, UV-Vis spectrophotometer, Transmission electron microscope (TEM), Scanning electron microscope (SEM), Energy dispersive spectroscopy (EDS). XRD shows the particles size with high crystallinity and purity which is in good agreement with the TEM result. The particles size of the synthesized TiO2 nanomaterial at calcination temperatures of 250oC, 400oC and 600oC were 9.22 nm, 14.33 nm and 36.72 nm respectively calculated from XRD result. The absorption edge for TiO2 nanomaterials synthesized by sol gel synthesis method was found to be 350 nm and the corresponding calculated band gap energy was 3.54 eV. The average particles size of the synthesized TiO2 nanopowder investigated from TEM using histograms at calcination temperatures of 250oC, 400oC and 600oC were found (8.55 ± 0.25) nm, (13.82 ± 0.41) nm and (36.06 ± 2.03) nm respectively. The polygonal structure of TiO2 nanomaterials were studied by scanning electron microscope. The EDS result showed that at calcination temperatures of 250oC, 400oC and 600oC, the concentrations of titanium were 33.34%, 32.6% and 31.89%, and the concentrations of chlorine were 2.64%, 0% and 0%, and the concentrations of oxygen were 64.02%, 67.4% and 68.11% in the synthesized TiO2 nanopowder respectively which is qualitatively confirmed by energy dispersive x-ray spectroscopy results.