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Formation and Characterisation of Cdse-Tio2 Nanoparticle Films By Formation and Characterisation of CdSe-TiO2 Nanoparticle Films by Electrophoretic Deposition KHATIJAH AISHA YAACOB A thesis submitted to Imperial College London in fulfillment of the requirements of the degree of Doctor of Philosophy and for the Diploma of Imperial College London Department of Materials Imperial College London Abstract Electrophoretic deposition (EPD) was used to form a composite layer of mercaptoundeconic acid (MUA) capped CdSe-TiO2 nanoparticle on a fluorine doped indium tin oxide (FTO) substrate. The CdSe-TiO2 layer can be employed to fabricate a quantum dot sensitized solar cells (QDSSC), increased contact between CdSe and TiO2 nanoparticles and leading to improved efficiency of the solar cells. A colloidal suspension of TOPO capped CdSe nanoparticles was prepared by the hot injection method, followed with ligand exchange in order to produce MUA capped CdSe nanoparticles. CdSe particle of diameter in the range of 2.44 nm to 3.26 nm were to be used in this research. The TiO2 nanoparticles were prepared by hydrolysis of titanium isopropoxide in water and produced particles size of 4.66 nm. Both nanoparticles were suspended in ethanolic medium. Electrophoretic deposition parameters were optimized. The results show that an applied voltage of 5 V, was suitable to be used to deposit single layer of MUA capped CdSe, TiO2 nanoparticles and the mixture of MUA capped CdSe-TiO2 nanoparticles. Smooth, uniform and dense layer were produced under this applied voltage. EPD also allows deposition of multilayer structures, in this research two layer structures of MUA capped CdSe on electrophoretically deposited TiO2 on FTO and mixed MUA capped CdSe-TiO2 on electrophoretically deposited TiO2 on FTO were formed. Three layer structures of MUA capped CdSe/MUA capped CdSe-TiO2/ TiO2/FTO were also synthesised. The photocurrent was measured on single layer, two layer and three layers electrodes. The optimum photocurrent parameters for each single layer were studied, in order to measure the photocurrent at the best condition possible. The highest IPCE value recorder was 0.70 % on MUA capped CdSe on FTO, with the MUA capped CdSe size of 2.94 nm. The lowest IPCE, 0.011 %, was obtained from three layer structure of MUA capped CdSe/MUA capped CdSe-TiO2/ TiO2/FTO. 1 Acknowledgements I would like to express my sincere gratitude: To my supervisor Dr Jason Riley for the initial idea, all his guidance and support during these studies. To all members of Electrochemistry Group in Department of Materials, Imperial College London. To the staff of the Harvey Flower Microstructural Characterisation Suite Imperial College London for the help in SEM study. To my sponsors the Ministry of Higher Education Malaysia and Universiti Sains Malaysia for the financial assistance during my study at Imperial College. To my husband Rashidi and my daughter Hannah, for their unmitigated love, encouragement, patience and understanding for all these years. This Thesis is the result of your sacrifices and for which I will never repay. 2 Declaration of Originality This Thesis is account of the work carried out between October 2007 and April 2011 at Imperial College London under the supervision of Dr. Jason Riley. I declare that this work was carried out in accordance with the Regulations of Imperial College London. The work is original except where indicated by special reference in the text and no part of the thesis has been submitted for another degree. This Thesis has not been presented to any other University for examination either in the United Kingdom or overseas. Signature: Dated: 3 Table of Contents Abstract 1 Acknowledgements 2 Declaration of Originality 3 List of Figures 10 List of Tables 17 List of Abbreviations 18 List of Symbols 20 Chapter 1 Introduction 22 1.1 Introduction 22 1.2 Aims of the Research 25 1.3 Outline of the Thesis 27 Chapter 2 Literature Review 28 2.1 Semiconductor Nanoparticles 28 2.1.1 Quantum Confinement in Semiconductor Nanoparticles. 29 2.2 CdSe Nanoparticles 30 2.3 Properties of CdSe Nanoparticles 32 2.3.1 Optical Properties of CdSe 32 2.3.1.1 Band Gap Calculation for CdSe Nanoparticles 33 2.4 Colloid Synthesis of Semiconductor Nanoparticles 35 2.4.1 Aspects of Nanoparticles Growth in Colloidal Solutions 35 2.4.1.1 Ostwald Ripening 36 2.4.2 Colloid Synthesis of CdSe Nanoparticles 37 2.4.3 Semiconductor Nanoparticles Synthesised by the Organometallic Route 39 2.4.4 Semiconductor Nanoparticles Synthesised in Aqueous Precipitation 40 2.4.5 Applications of CdSe Nanoparticles in Optoelectronic Devices 42 4 2.5 Metal Oxide Nanoparticles 42 2.6 TiO2 Nanoparticles 44 2.6.1 Crystal Structure 44 2.6.2 Properties of TiO2 46 2.6.2.1 Electrical Properties 46 2.6.2.2 Optical Properties 47 2.6.2.3 Band Gap Calculation for TiO2 Nanoparticles 47 2.6.3 Synthesis of TiO2 48 2.6.3.1 Sol Gel Synthesis Parameters 50 2.6.4 Application of TiO2 in Energy Conversion 53 2.6.4.1 Photoelectrochemical Cell (PEC) 53 2.6.4.2 Photovoltaic Solar Cells 54 2.7 Electrophoretic Deposition (EPD) 57 2.7.1 The EPD Process 58 2.7.2 Charge on Particles 60 2.7.3 Factors That Affect the EPD Process 61 2.7.3.1 Colloidal Properties of Suspension 62 2.7.3.2 EPD Process Parameter 65 2.7.4 Co-Deposition of EPD 68 2.7.5 Modelling of the EPD Process 69 2.7.6 Application of EPD 70 2.7.7 EPD of CdSe Nanoparticles 71 2.7.8 EPD of TiO2 Nanoparticles 73 Chapter 3 Experimental Techniques 75 3.1 Electrophorectic Deposition (EPD) 75 3.1.1 Preparation of Electrodes 75 3.1.2 Electrodes Cleaning Procedure 75 3.1.3 Electrode Configuration 76 3.1.3.1 EPD of TOPO Capped CdSe 76 3.1.3.2 EPD of MUA Capped CdSe and TiO2 Nanoparticle 77 3.2 Optical Properties 78 3.2.1 UV Visible Spectroscopy 78 3.2.2 Photoluminescence (PL) Spectroscopy 80 3.3 Transmission Electron Microscopy (TEM) 81 5 3.3.1 Focus Ion Beam (FIB) 82 3.4 Scanning Electron Microscopy1 82 3.5 X-Ray Diffraction (XRD) 83 3.5 White Light Interferometer (Zygo®) 84 3.6 Inductive Couple Plasma-Optical Emission Spectroscopy (ICP-OES) 85 3.7 Zeta Potential Measurement 85 3.8 Photocurrent Spectroscopy 87 3.8.1 Photocurrent Measurement Apparatus 89 3.8.2 The Electrochemical Cells 90 3.8.3 Calibration 91 3.8.4 Calculation of the IPCE (Incident Photon-to-Current Efficiency) 92 3.8.5 Band Gap Calculation from IPCE 93 Chapter 4 Synthesis of the Nanoparticles 94 4.1 Synthesis of CdSe Nanoparticles 94 4.1.1 Chemicals 94 4.1.2 Synthesis of TOPO Capped CdSe Nanoparticles 94 4.1.3 Optical Properties of the TOPO Capped CdSe 96 4.1.3.1 The Effect of the HDA and TDPA to the Synthesis of CdSe Nanoparticles 97 4.2 Purification of CdSe Nanoparticles Solution by Repeated Precipitation 101 4.2.1 Optical Properties of Washed CdSe 102 4.2.2 TEM 105 4.2.3 ICP 108 4.3 Ligand Exchange 109 4.3.1 MUA Capped CdSe nanoparticles by Peng et al. (199) 110 4.3.1.1 Optical Properties of MUA Capped CdSe 111 4.3.1.2 TEM 113 4.4 Synthesis of TiO2 Nanoparticles 114 4.4.1 Chemicals 115 4.4.2 Kamat et al. (77) and Srikanth et al. (97). 115 4.4.3 New Method for the Synthesis of TiO2 Nanoparticles 118 6 4.4.3.1 Characterization/Analysis 118 Chapter 5 Results and Discussions 121 5.1. EPD of TOPO Capped CdSe 121 5.1.1 Instrument and Method 121 5.1.2 EPD Parameters Related to the Processing of TOPO Capped CdSe 122 5.1.2.1 Applied Voltage during EPD of TOPO Capped CdSe Suspension 123 5.1.2.2 Deposition Time of TOPO Capped CdSe for 30 minute 126 5.1.2.3 Electrode Gap during EPD of TOPO Capped CdSe 128 5.1.3 Surface Morphology of TOPO Capped CdSe Film 130 5.2 EPD of MUA Capped CdSe 132 5.2.1 Instrument and Method 132 5.2.2 EPD Parameters Related to the Processing of MUA Capped CdSe 134 5.2.2.1 Applied Voltage during EPD of MUA Capped CdSe Suspension 134 5.2.2.2 pH of MUA Capped CdSe Suspension 135 5.2.2.3 Purification of MUA Capped CdSe Suspension 136 5.2.2.4 Deposition Time of MUA Capped CdSe Suspension 139 5.2.2.5 Silanisation of the FTO Electrodes 142 5.2.2.6 Summary Related to EPD Parameters of MUA Capped CdSe Suspension 144 5.2.3 Behaviour of Deposition Current During EPD of MUA Capped CdSe 144 5.2.4 Sintering Effect of MUA Capped CdSe Films 145 5.2.5 Surface Morphology of MUA Capped CdSe Films 147 5.3 EPD of TiO2 148 5.3.1 Instrument and Method 149 5.3.2 EPD Parameters Related to the Processing of TiO2 Nanoparticles 149 5.3.2.1 Apparent pH of TiO2 Nanoparticle Suspension 150 5.3.2.2 Applied Voltage during EPD of TiO2 Nanoparticle Suspension 151 5.3.2.3 Solid Concentration of TiO2 Nanoparticle Suspension 152 5.3.2.4 Deposition Time of TiO2 Nanoparticle Suspension 153 5.3.2.5 Summary Related to EPD Parameters of TiO2 Nanoparticle Suspension 154 5.3.3 Behaviour of Deposition Current During EPD of TiO2 Nanoparticles 155 5.3.4 Sintering Effect of TiO2 Nanoparticle Films 156 5.4 Electrophoretic Co-deposition of CdSe-TiO2 Nanoparticle 159 5.4.1 Instrument and Method 160 7 5.4.2 Zeta Potential Measurement of Mixed MUA Capped CdSe-TiO2 Nanoparticle Suspension 160 5.4.3 Deposition Time of CdSe-TiO2 Nanoparticle Suspension 161 5.4.4 Behaviour of Deposition Current During EPD of CdSe-TiO2 Nanoparticle 163 5.5 Photocurrent Measurements 163 5.5.1 Photocurrent Measurement of TOPO Capped CdSe/FTO 166 5.5.1.1 Discussion on Photocurrent Measurement of TOPO Capped CdSe 166 5.5.2 Photocurrent Measurement of MUA capped CdSe/FTO 168 5.5.2.1 Frequency Dependence of IPCE 168 5.5.2.2 The pH of Electrolyte 169 5.5.2.3 Potential of the Cell 171 5.5.2.4 Effect of Deposition Time of MUA Capped CdSe on IPCE 172 5.5.2.5 Sintering Effect on Band Gap 175 5.5.3 Photocurrent Measurement of TiO2/FTO 177 5.5.3.1
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