Titanium Dioxide Films Prepared by Sol-Gel/Laser-Induced Technique for Inactivation of Bacteria

  • Yasir Joya

Student thesis: Phd

Abstract

In the present research, a novel method, namely sol-gel/laser-induced technique (SGLIT), has been developed to generate nano-structured TiO2-based films. The TiO2 films based on unloaded (pure) TiO2, Ce-TiO2, W-TiO2 and Ag-TiO2, have been investigated in attempt to stabilise the formation of anatase and consequently of enhancing photo-catalytic and anti-bacterial activities. The TiO2 precursor loaded with Ce2+, W6+ and Ag2+ ions (Ce-TiO2, W-TiO2 and Ag-TiO2) were separately prepared by sol-gel method and spin-coated on microscopic glass slides. A pulsed KrF excimer laser with a wavelength of 248 nm and pulse width of 13-20 ns was employed to irradiate on the sol-gel prepared films at various operating parameters, in terms of laser fluence, number of laser pulses and repetition rate. The work has been focussed on microstructural characterisation of various films prepared by both SGLIT and furnace, in the consideration of crystallographic structure, phase transformation, crystallite sizes, surface morphology, film thickness and optical properties, by means of Raman spectroscopy, XRD, FEG-SEM/EDX, TEM/HR-TEM/EDX, AFM and UV-Vis spectroscopy etc. The results showed that nano-crystallisation of the films after laser irradiation has been achieved, with controllable amount of anatase formation. These coatings presented a unique feature of surface morphology with meso-porosity and much enlarged surface areas, compared with the films prepared by furnace sintering technique. The addition of Ce and Ag, stabilized the anatase structure during the laser irradiations, whereas the addition of W destabilized the anatase structure. The Ce-TiO2 films prepared by SGLIT exhibited anatase structure which was stable up to 500 laser pulses at 35 mJ cm-2 fluence. The anatase was formed after 10 laser pulses only at 65-75 mJ cm-2 fluence in the W-TiO2 films. When a higher number of laser pulses, fluence or higher W6+ loading were chosen, rutile structure started to form. On the other hand, the Ag-TiO2 nano-composite films prepared by SGLIT presented the anatase up to 200 laser pulses at 85 mJ cm-2 fluence. On average, anatase crystallite size of about 38 nm was achieved from both the W-TiO2 and Ag-TiO2 films prepared by SGLIT. In contrast, the furnace-sintered W-TiO2 and Ag-TiO2 films produced anatase crystallite size of 49.4 nm and 29.8 nm respectively. Another achievement of the present research is the development of a single-step laser irradiation technique to generate an Ag-TiO2 nano-composite film on the glass substrate. A pulsed laser beam produced hexagonal Ag nanoparticles along with the crystallization of anatase-based nano-structured TiO2 film which was accomplished in 1 µs only. The films prepared by SGLIT displayed a higher photo-absorption compared to their furnace-sintered counterparts due to the unique surface features with a higher surface roughness. Overall, an enhanced bactericidal activity against E. coli cells was demonstrated under UV light by each of the W-TiO2 films compared to furnace-sintered films except the 1W-TiO2. The E. coli cells did not survive on the W-TiO2 films prepared by SGLIT, after 80 minutes under UV (365 nm) light. In contrast, E. coli cells still survived on the surface of furnace-sintered W-TiO2 films under the same conditions. Ag-TiO2 nano-composite films prepared by SGLIT, demonstrated an enhanced anti-bacterial activity against E. coli compared to the conventionally- made Ag-TiO2 films. No bacteria survived on the Ag-TiO2 films prepared by 50 laser pulses at 85 mJ cm-2 fluence, whereas E. coli colonies always survived on the furnace-sintered Ag-TiO2 films under the UV, natural light and the dark room conditions.
Date of Award1 Aug 2011
Original languageEnglish
Awarding Institution
  • The University of Manchester
SupervisorZhu Liu (Supervisor)

Keywords

  • XRD
  • TEM
  • Excimer laser
  • FEG-SEM
  • Analytical Modeling
  • Laser processing
  • Sol-gel
  • Titanium dioxide
  • E-Coli

Cite this

'