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The Synthesis, Characterisation and Application of Transparent Conducting Thin Films

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The Synthesis, Characterisation and Application of Transparent Conducting Thin Films The Synthesis, Characterisation and Application of Transparent Conducting Thin Films This thesis is submitted in partial fulfillment of the requirements for the Degree of Doctor of Engineering (Chemistry). Mathew Robert Waugh University College London 2011 i I, Mathew Robert Waugh, confirm that the work presented in this thesis is my own. Where information has been derived from other sources, I confirm that this has been indicated in the thesis. This thesis is dedicated to „the Champ‟. ii Abstract Transparent conducting thin films of metal oxides, doped metal oxides, and carbon nanotubes (CNTs), have been produced using various deposition techniques, including: Aerosol Assisted Chemical Vapour Deposition (AACVD), Atmospheric Pressure Chemical Vapour Deposition (APCVD), and Spray Coating. The resultant thin films were tested for their performance in a number of applications, including: Low emissivity (‘Low-E’) glazing, photovoltaic electrode materials, gas sensing and photocatalysis. AACVD was shown as a viable, and attractive, deposition technique for the synthesis of tin oxide, and doped tin oxide thin films, which allows for controllable doping levels, crystallinity, and surface structure. The tailoring of these physical attributes allows for enhanced performance of the functional properties of the films, whereby, a lower growth temperature produced highly transparent, highly conductive coatings with a low haze value for ‘Low-E’ applications, whereas, higher growth temperatures produced the high electrical conductivity, transparency, and light scattering properties required for high performance electrodes in thin film photovoltaics. In addition, a dual coating methodology was developed using both AACVD, and APCVD, to grow tin oxide thin films in a rapid timescale, but with modified surface structures showing changes to the short range waviness, kurtosis, and the surface area. Growth of carbon nanotubes, using CVD, was investigated over a range of metal catalysts, with varying Pauling electronegativity values, and over a range of temperature, methane, and hydrogen conditions. A growth mechanism has been postulated, whereby, the electronegativity of the metal catalyst, and the solubility and diffusion of the carbon through that catalyst, affects the type and properties of the carbon structure produced. To the authors knowledge, this is the first reported growth of MWCNTs using a chromium solo-metal catalyst, and the first reported growth of the unique ‘carbon nanofibres’ which were produced using gold and silver metal catalysts. iii Functionalisation of SWCNTs using a microwave reflux process was shown to yield sulphonate and sulphone modified nanotubes, which are highly soluble in water and able to undergo spray coating to produce carbon nanotube, nanonet transparent conducting thin films. The functionalisation process was shown to be reversible upon heating of the modified nanotubes. AACVD has been deemed unable to produced doped zinc oxide transparent conducting films. However, undoped zinc oxide films were produced. They displayed a high photocatalytic action in the degredation of stearic acid, and a UV light induced superhydrophilicity. The modification and deposition techniques, established throughout this work, were utilised to form transparent, hybrid, metal oxide-CNT coatings, for gas sensing. The hybrid materials displayed enhanced response times to combustible target gases, which has been attributed to the catalytic effects of the exposed carbon nanotube surfaces; and to the spillover of adsorbed oxygen from the active nanotubes to the metal oxide surface. iv Acknowledgements I would like to thank my supervisor, Professor Ivan P. Parkin, for his guidance, encouragement and the countless opportunities he has presented to me over the course of my doctorate: I couldn’t have asked for a better supervisor or a nicer person, who has a genuine desire to cultivate creative science, and benefit society through the field in which he excels. I would also like to thank: my secondary supervisor, Professor Claire Carmalt, for all her help; Dr Troy Manning and Senior Technologist Simon J. Hurst, of Pilkington NSG, for finding time in their busy schedules to help foster a better dialogue between academia and industry alongside all the personal guidance and wisdom they have selflessly passed on to me. My acknowledgements page would not be complete, without passing on in most instances my deepest gratitude, and in others my unwavering sympathy, to the lecturing staff, technicians, postdocs and students, who showed me the ropes, gave me (mostly) sound advice and put up with my mood swings. My special thanks goes out to: Dr Chris Blackman, Dr Russell Binions, Dr Andrea Sella, Dr Steve Firth, Kevin Reeves, Dave Knapp, Crosby Medley, Dr Geoffrey Hyatt, Dr Charlie Dunhill, Dr Caroline Knapp, Dr Luanne Thomas (with whom I shared my doctoral torment), Dr Kris Page, Davinda Bachu, Savio Moniz, Paulo Melgari, Ayo Alfonja, Teegan Thomas, Leanne Bloor, Ralph Leech and the countless others who have helped me along the way. Last, but by no means least, I want to say a massive thank you to all my family and friends who have supported, encouraged and humoured me, in all of my endeavours. Extra special gratitude goes to my parents; to Jessie and Jim; to Pete and the guys; to my grandparents; to Eddie, Asha and Lorna; to Waltbot, Lingbot, Stringbot, Jack Johnson, Wiggles, Jimbles, Sweet-Pea and Mr Breaks; to Keith, Glynis and Campo; and especially to Charlotte Louise Hampshire, I couldn‟t have done it without you. v ……“Learn from yesterday, live for today, hope for tomorrow. The important thing is not to stop questioning.” Albert Einstein. ……“Stupid is as stupid does.” Forest Gump. vi List of Analytical Techniques: Atomic Force Microscopy analysis was performed using a Veeco Dimension 3100 in intermittent contact mode using a cantilever and tip under resonant frequency. Analysis was done using Gwyddion 2.14 freeware. Crystallite Size was determined from the XRD patterns using the Scherrer equation1, 2. The full width at half maximum standard used was a 25 cm2 alumina flat plate obtained from the National Institute of Standards and Technology (NIST), with peak intensities given by NIST and peak positions by the ICDD. Diffuse Transmittance measurements were done on a JASCO V-570 UV/VIS/NIR spectrophotometer by deducting direct transmittance spectra from the total transmittance spectra (using direct transmittance and optical integrating sphere modes to capture the two spectra respectively) to yield a % diffuse transmittance spectra. Hall effect measurements were carried out using the Van Der Pauw method3, to determine the sheet resistance, free carrier concentration (N) and mobility (µ). A square array of ohmic contacts arranged on a 1 cm2 sample with a calibrated magnetic field was used. Haze Measurements were performed using a BYK Gardner haze-gard plus, operating over the CIE luminosity function y visible spectral range. Infrared Spectroscopy was performed using a Perkin Elmer FT-IR spectrum RXI spectrometer over a wavenumber range of 500 cm-1 to 4000 cm-1. vii Raman Spectroscopy was performed using a Renishaw invia Raman microscope at 514.5 nm and 785 nm (green and red lasers respectively). The operating power was set between 1 and 5 % to avoid radiative degradation of the samples. Scanning Electron Microscopy and Energy Dispersive Elemental Analysis SEM was performed using a JEOL JSM-6301F Field Emission SEM at an accelerating voltage of 5 keV. EDXA was performed using an attached Oxford Instruments INCA Energy EDXA system. Sheet Resistance measurements were recorded using an ‘in house set-up’ linear four point probe. Thermo-Gravimetric Analysis was done on a NETZSCH STA–449C Jupiter balance under helium flow, up to a temperature of 1500˚C. Transmission Electron Microscopy (High Resolution) Transmission Electron Microscopy (TEM) was completed using a JEOL JEM-4000EX HRTEM at 100 kv. Transmission Electron Microscopy and Electron Diffraction were performed using a JEOL JEM-100CX 2 microscope at an accelerating voltage of 100 kv. UV/Visible Absorption Spectroscopy was performed using a Perkin Elmer Lambda 25 spectrometer over 250 – 900 nm. viii UV/Visible/Near IR spectra were taken using a Perkin Elmer Fourier transform Lambda 950 UV/Vis spectrometer over a wavelength range of 300 nm to 2500 nm in both transmission and reflection modes. Wavelength Dispersive X-ray was used to quantify thin film atomic ratios using a Phillips XL30 E-SEM and Oxford instruments INCA Energy detector. X-ray Diffraction measurements, to analyze crystallinity and orientation of the samples, were completed using a Bruker D8 X-ray diffractometer with CuKα1 and CuKα2 radiation of wavelengths 0.154056 nm and 0.154439 nm respectively, emitted with an intensity ratio of 2:1, a voltage of 40 kV and current of 40 mA were used. The diffraction pattern was taken over 10-70º 2θ. ix Contents 1 Introduction ................................................................................. 1 1.1 Thesis Overview .............................................................................................. 1 1.2 Transparent Conducting Materials ................................................................... 3 1.3 Thin Film Deposition Techniques ...................................................................... 4 1.3.1 Wet Chemical .................................................................................................... 5 1.3.2 Physical Vapour deposition
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