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Single and Double Doping of Nanostructured Titanium Dioxide with Silver And

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Single and Double Doping of Nanostructured Titanium Dioxide with Silver And Single and Double Doping of Nanostructured Titanium Dioxide with Silver and Copper: Structural, Optical and Gas-Sensing Properties by NUBI OLATUNBOSUN OWOLABI THESIS Submitted in fulfilment of the requirements for the degree of DOCTOR OF PHILOSOPHY in PHYSICS in the FACULTY OF SCIENCE & AGRICULTURE (School of Physical and Mineral Sciences) at the UNIVERSITY OF LIMPOPO PROMOTER: Prof. K.E. Rammutla CO-PROMOTER: Dr. T.E. Mosuang 2016 Dedications This one is for you, my late parents. A little too late perhaps, but I got there in the end: Baba, Mama: Bawo ni iba ti dun mo mi ninu to kani e wa laye. Mo dupe pupo lowo yin nitoriwipe e ko fi mi sile. E duro timi titi e fi fi aiye sile. Nitori eyi ni mo fi da lokan wipe mo ma yonju eleyi, yala ohun to o ma gba. E sun re o. i Declaration I declare that SINGLE AND DOUBLE-DOPING OF TITANIUM DIOXIDE NANOPARTICLES WITH SILVER AND COPPER: STRUCTURAL, OPTICAL AND GAS-SENSING APPLICATIONS hereby submitted to the University of Limpopo, for the degree of Doctor of Philosophy (Physics) has not previously been submitted by me for a degree at this or any other university; that it is my work in design and in execution, and that all material contained herein has been duly acknowledged.. ………………………………………………………………………………………………….. NUBI OO (Mr) Date ii Acknowledgements The synthesis of the nanostructured titanium dioxide samples studied in this research was primarily carried out in the laboratories of the University of Limpopo. Other experimental facilities, particularly those involving sample characterisation, were made available through collaboration with other research centres. For financial and equipment support we acknowledge: University of Limpopo (UL) National Research Foundation (NRF) Centre for Scientific and Industrial Research (CSIR) Department of Science and Technology (DST) India-Brazil-South Africa (IBSA) Academic/research support, supervision and guidance: Prof Erasmus Rammutla (RIP God-sent) Dr Thuto Mosuang Dr Bonex Nwakikunga Gratitude Statement: God made. Papa moulded. Mama nurtured. Wife persevered. Children endured. Uncle insisted. Friends supported. Existence is priceless! I am really very grateful. iii Abstract Single and double doped nanometric powders of titanium dioxide (TiO2) were synthesised by the sol-gel process using titanium isopropoxide (TTIP) as the precursor. For comparison, an undoped sample was also prepared. The metal dopants, Ag and Cu, were used at doping levels of 5% molar weight. The samples were dried at 100°C in air and post annealing was done at 300°C, 600°C, 900°C and 1100°C. Structural characterisation of the samples was carried out by X-ray Diffraction (XRD), Raman Spectroscopy, Scanning Electron Microscopy (SEM) and Energy dispersive X-ray Spectrometry (EDS) techniques. Most samples annealed at the 300°C temperature (and lower) revealed the predominantly-anatase phase, while those annealed at 900°C and above were rutile-only. The double-doped powder that was annealed at 300°C was found to be constituted by anatase and brookite phases (with the dopants incorporated into the TiO2 matrix), and the one annealed at 600°C was a mixture of brookite and rutile. The results suggest that multiple doping of titania may favour a two-phase structure at lower temperatures than singly-doped powders. The co-existence of brookite with anatase is believed to be responsible for the enhancement of anatase to rutile transformation in the double-doped sample. UV-visible (UV-vis) and Photoluminescence (PL) measurements were also carried out to study the optical properties of the TiO2 nanoparticles. This revealed the active PL band at around 440 nm. By narrowing the band gap, the double-doped powders that exhibited the brookite phase, again showed improved visible light photo absorption over the other samples, with a significant shift of the absorption edge to shorter wavelengths. Further, PL spectra revealed a change in PL intensity with phase change, as well as the presence of exciton energy levels at the base of the conduction band. The changes in the electrical conductivities of representative anatase and rutile TiO2 nanopowders upon exposure to water-vapour, ammonia (NH3) and hydrogen (H2) were also investigated. Sensing measurements for water-vapour was done at room temperature for various humidity levels ranging from 5.4% RH to 88.4% RH. The detection of NH3 and H2 gases were carried out at temperatures extending from room temperature to 350°C and over concentration ranges of 25 sccm to 500 sccm and 15 iv sccm to 200 sccm respectively. The gas-sensing results show that the sol-gel fabricated TiO2 nanoparticles (particularly in anatase form), has excellent fast and stable dynamic responses to humidity, NH3 and H2. They feature good sensitivities, even at a low operating temperatures. However, acceptor behaviour, for which there was a conductivity switch from n-type to p-type, was recorded for the Ag-doped rutile powders at operating temperatures of 300ºC and 350ºC. Overall, the double-doped sample annealed at 300ºC was deemed the most promising candidate for gas- sensing. Ni Soki… TiO2 bintin je atikun ti o se pataki ni orisirisi ona, papa julo ti a ba fi silifa ati kopa die- die kun lapapo. v Table of Contents Dedications ................................................................................................................... i Declaration .................................................................................................................. ii Acknowledgements .................................................................................................... iii Abstract ...................................................................................................................... iv List of Tables .............................................................................................................. xi List of Figures ........................................................................................................... xiii 1. BACKGROUND ................................................................................................... 1 1.1 INTRODUCTION ........................................................................................... 2 1.1.1 Resent Research .................................................................................... 2 1.1.2 Key concepts .......................................................................................... 4 1.2 RESEARCH PROBLEM ................................................................................ 4 1.2.1 Source and Background of the Problem ................................................. 4 1.2.2 Statement of the Research Problem ....................................................... 5 1.3 LITERATURE REVIEW ................................................................................. 5 1.4 PURPOSE OF THE STUDY .......................................................................... 6 1.4.1 Research Aim ......................................................................................... 6 1.4.2 Hypothesis .............................................................................................. 6 1.4.3 Specific Objectives .................................................................................. 6 1.5 RESEARCH METHODOLOGY ..................................................................... 7 1.6 SIGNIFICANCE OF PROPOSED RESEARCH ............................................. 7 1.7 SCOPE, LIMITATIONS AND DELIMITATIONS OF THE STUDY ................. 8 1.8 DISSERTATION OUTLINE ........................................................................... 9 2. FUNDAMENTALS & LITERATURE REVIEW .................................................... 10 2.1 INTRODUCTION ......................................................................................... 11 2.2 RESEARCH IN NANOTECHNOLOGY ........................................................ 12 2.3 SCIENTIFIC REVIEWS ON NANOSTRUCTURED TITANIUM DIOXIDE ... 14 vi 2.4 NANOPARTICLES AND NANOPOWDERS ................................................ 14 2.5 PROPERTIES OF NANOSTRUCTURED TITANIA ..................................... 17 2.5.1 Structural Properties of Nanosized Titania ............................................ 17 2.5.2 Thermodynamic Properties of Nanosized Titania ................................. 20 2.5.3 X-ray Diffraction Properties of Nanosized Titania ................................. 22 2.5.4 Raman Vibration Properties of Nanosized Titania ................................ 25 2.5.5 Electronic Properties of Nanosized Titania ........................................... 26 2.5.6 Optical Properties of Nanosized Titania ................................................ 30 2.5.7 Photon-Induced Electron & Hole Properties of Nanosized Titania ........ 33 2.5.8 Gas Sensing Properties of Nanosized Titania....................................... 34 2.6 SYNTHESIS OF TITANIA NANOSTRUCTURES ........................................ 45 2.6.1 The Sol-Gel Method .............................................................................. 45 2.6.2 Non-Hydrolytic Sol Method ................................................................... 49 2.6.3 Micelle and Inverse Micelle Methods .................................................... 52 2.6.4 Hydrothermal Method ........................................................................... 54 2.6.5 Solvothermal Method ............................................................................ 57 2.6.6 Direct Oxidation Method ......................................................................
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