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Title Page

Abstract

Contents

Chapter 1: Introduction 15

References 19

Chapter 2: Synthesis of Transition Metal Oxides Nanostructures 21

2.1. Introduction 21

2.2. Solvothermal Synthesis of Metal Oxides Nanostructures 23

2.3. Sol-Gel Synthesis of Metal Oxides Nanostructures 25

2.4. Electrochemical Synthesis of Metal Oxides Nanostructures 27

2.5. Hydrothermal Synthesis of Metal Oxides Nanostructures 28

2.6. Hydrothermal Synthesis of MoO₃ and Cu0.33MoO₃ Nanowires(이미지참조) 32

2.7. Hydrothermal Synthesis of MoO₃-MWCNTs Nanocomposites 33

2.8. Conclusion 34

Reference: 35

Chapter 3: Structural Characterization of Transition Metal Oxides Nanostructures 40

3.1. Introduction 40

3.2. X-ray diffraction (XRD) 41

3.3. Raman Spectroscopy 45

3.4. Field Emission Scanning Electron Microscopy (FE-SEM) 49

3.5. Transmission Electron Microscopy (TEM) 54

3.6. Energy Dispersive X-ray Spectroscopy (EDS) 58

3.7. X-ray photoelectron spectroscopy (XPS) 60

3.8. UV- Visible spectroscopy 63

3.9. Conclusion 65

Reference 68

Chapter 4: Design of Electrode for Electrochemical Energy Storage and Conversion Devices using Molybdenum Oxide Nanowires 74

4.1. Introduction 74

4.2. Experimental Section 75

4.2.1. Electrode Fabrication 75

4.3. Electrochemical Characterization of MoO₃ Nanowires for Energy Storage Devices 76

4.3.1. Charge Storage Mechanism in MoO₃ Nanowires 78

4.4. Electrochemical Characterization of MoO₃ Nanowires for Biological Applications 83

4.4.1. Functionalization of Nanowires 83

4.4.2. Effect of pH of Buffer Solution on the response of the Biosensor 84

4.4.3. Role of MoO₃ Nanowires in Electron Transfer 86

4.4.4. Chronoamperometric Response and Calibration Curve 90

4.4.5. Reproducibility and Long-term Stability of the Biosensor 91

4.5. Photocatalytic Characterization of MoO₃ Nanowires for Energy Conversion Devices 94

4.6. Possible Photodegradation Mechanism 100

4.7. Conclusion 104

References 106

Chapter 5: Electrochemical High Performance and Stable Energy Storage Devices Based on Intertwined Porous MoO₃-MWCNTs Nanocomposites 111

5.1. Experimental Section 111

5.2. Preparation of Working Electrode 112

5.3. Electrochemical Characterization of MoO₃-MWCNTs Nanocomposites for Energy Storage Devices 112

5.4. Electrochemical Impedance Measurements 120

5.5. Raman and TEM Analysis after Cycling 122

5.6. Photocatalytic Characterization of MoO₃-MWCNTs Nanocomposites for Energy Conversion Devices 124

5.7. Conclusion 130

Reference: 132

Chapter 6: Conclusions and Future Work 134

List of Tables

Table 1: Possible interferences from other substrates for lactate determination (0.05 M phosphate buffer at pH 7) 94

Table 2: Surface area, pore volume and average pore diameter of the different catalysts 103

Table 3: Comparison of photocatalytic properties of TiO₂ and our samples 103

List of Figures

Figure 2-1: (a-d) Photographs of a standard laboratory oil bath on a hot plate with stirrer, flask and reflux condenser, (b) Parr autoclave, (c) microwave oven, and (d) microwave reaction tube. 24

Figure 2.2: Schematic representation of the condensation between Ti-OiPr and Ti-Cl catalyzed by TiCl₃OiPr. 27

Figure 2-3: Phase diagram of water. 29

Figure 2-4: Schematic of an autoclave used for the synthesis of metal oxide nanostructure. 30

Figure 3-1: Schematic of Bragg’s reflection from a crystal. 42

Figure 3-2: (a) XRD patterns of MoO₃ nanowires; (I) 120℃, (II) 150℃, (III) 180℃; (b) XRD patterns of MoO₃ nanowires: (I) 180℃, (II) Cu0.33MoO₃ nanowires at 180℃. The as-synthesized MoO₃-MWCNTs nanocomposites were also examined by X-ray diffraction. Figure 3-3 shows the XRD pattern of MoO₃-MWCNTs composite. The...(이미지참조) 44

Figure 3-3: XRD patterns of MoO₃ nanowires MoO₃-MWCNTs nanocomposite synthesized at 180 ℃ for 6 hours (where unlabeled peaks represents the carbon peaks). 45

Figure 3-4: (a) Raman spectrum of MoO₃ nanowires, (b) MoO₃-MWCNTs nanocomposite 49

Figure 3-5: (a) FE-SEM image of MoO₃ nanowires synthesized at 120℃ for 12 hours (b) 150℃ for 12 hours (c) 180℃ for 12 hours (d) 210℃ for 12 hours. 53

Figure 3-6: FE-SEM images of (a) Cu doped MoO₃ nanowires (b) intertwined MoO₃-MWCNTs nanocomposite with 5% MWCNTs , (a) 10% MWCNTs, (b) 20% MWCNTs. 54

Figure 3-7: (a) TEM and SAED of MoO₃ nanowires synthesized at 120℃ for 12 hours, (b) TEM and SAED of MoO₃ nanowires synthesized at 180℃ for 12 hours, (c) TEM and SAED of Cu doped MoO₃ nanowires synthesized at 180℃ for 12 hours, 57

Figure 3-8: Illustration of the principle of EDX. 59

Figure 3-9: EDS analysis of (a) MoO₃ nanowires, (b) Cu doped MoO₃ nanowires. 60

Figure 3-10: XPS spectrum of the MoO₃ nanowires, MWCNTs, MoO₃-MWCNTs nanocomposite and Cu doped MoO₃ nanowires. 62

Figure 3-11: Illustrating the principle of UV-Visible spectroscopy. 65

Figure 4-1: (a) Comparison of cyclic voltammograms (CV) of different nanowire electrodes at a scanning rate of 20 mV/s, (b) CV of nanowires synthesized at 180 ℃ at different scanning rates, (c) specific capacitance variation of nanowires at different scan rates, and (d) specific capacitance variation of nanowires as a function of the... 78

Figure 4-2: (a) Galvanostatic charge discharge curves of nanowires at different current densities. (b) First few charge discharge cycles of nanowires at 1 mA/㎠. (c) Variation of specific capacitance at different current densities. (d) Ragone chart of the supercapacitor obtained from discharge curves measured at different constant current... 82

Figure 4-3: FTIR spectra of the following samples: (a) MoO₃ nanowires before enzyme immobilization, and (b) MoO₃ nanowires after LOx attachment.(이미지참조) 84

Figure 4-4: (a) Effect of pH on the response of Au-MoO₃-LOx-Nafion electrode at 0.5V in presence of lactate (1 mM) and 0.05M Phosphate buffered saline, and (b) Cyclic voltammograms obtained from the Au-MoO₃-LOx-Nafion electrode in the 10 mM PBS at different.(이미지참조) 85

Figure 4-5: Comparison of the cyclic voltammograms response of the (a) Au-LOx -Nafion electrode and (b) Au-MoO₃-LOx-Nafion electrode, in PBS and after the addition of 2mM lactate. The scan rate was 50 mV s-1.(이미지참조) 88

Figure 4-6: (a) Amperometric response of the Au-MoO₃-LOx-Nafion electrode at 0.5 V versus Ag/AgCl upon the addition of lactic acid into the 2 mM PBS solution at concentrations of 1, 2, 3, 5, 7, and 8 mM every 50 seconds, and (b) Calibration curve.(이미지참조) 91

Figure 4-7: (a) Sensitivity values measured on ten different MoO₃ nanowires electrodes in lactate concentration range 0.5-8 mM, and (b) The variation of amperometric response taken over two weeks of a MoO₃ nanowires electrode to addition of 2mM lactate. 93

Figure 4-8: The XPS analysis of the Cu0.33MoO₃ nanowires, (a) the XPS spectrum of Mo, (b) the XPS spectrum of Cu, (c) the XPS spectrum O1s of MoO₃. (d) O1s of Cu0.₃₃MoO₃.(이미지참조) 96

Figure 4-9: Diffuse reflectance absorption spectra of MoO₃ and Cu0.33MoO₃(이미지참조) 97

Figure 4-10: Photocatalytic study of MoO₃, Cu0.33MoO₃ nanowires, and bulk MoO₃ under (a) UV, (b).visible light irradiation, (c) Temporal Changes in TOC during TBO degradation (0.2mg/L), (d) Photocatalytic degradation of chlorobenzene.(이미지참조) 98

Figure 4-11: Photocatalytic study of MoO₃, Cu0.2MoO₃ nanowires, under UV (a) and visible light irradiation (b).(이미지참조) 100

Figure 4-12: Possible mechanism for the photodegradation of TBO under visible light. (A) TBO is absorbed at the surface of MoO₃ nanowires; (B) TBO absorbs visible light to induce the π-π* transition, the excited-state electrons then readily inject into the d-orbital (CB) of MoO₃; (C) the excited-state electrons react with adsorbed oxygen to...(이미지참조) 102

Figure 5-1: (a) Cyclic voltammograms (CV) of the MoO₃ nanowires, MWCNTs and MoO₃-MWCNTs nanocomposite electrodes at a scan rate of 20mV/s (b) Cyclic voltammograms (CV) of MoO₃ nanowire (c) MWCNTs (d) MoO₃-MWCNTs nanocomposite electrodes at various scan rates from 5 to 100mV s-1 in a 1 M aqueous...(이미지참조) 114

Figure 5-2: (a) Specific capacitance variation of the MoO₃ nanowires, MWCNTs and MoO₃-MWCNTs nanocomposite electrodes at different scan rates (b) Cyclic voltammetry of the first and after 2000 cycles of MoO₃-MWCNTs composite (scan rate was 20 mV/s), (C) Galvanostatic charge-discharge curves of the MoO₃ nanowires,... 117

Figure 5-3: (a) Ragone chart of MoO₃ nanowires, MWCNTs and MoO₃-MWCNTs electrodes obtained from the discharge curves measured at different constant current densities, (b) Nyquist plot of the MoO₃ nanowires, MWCNTs and MoO₃-MWCNTs electrodes in the frequency regime from 100 kHz to 0.1 mHz, (c) Bode plot from the... 119

Figure 5-4: Raman spectra of MoO₃-MWCNTs recorded at 514 nm excitation after 100, 500, 1000 and 2000 voltammetric cycles (b) Increase of the ID/IG ratio for MWCNTs with the number of cycles, indicating the structural changes 123

Figure 5-5: HRTEM image of MoO₃-MWCNTs nanocomposite (a) after 1000 and (b) 2000 voltammetric cycles. The electron diffraction patterns (insets) show a loss of structural order due to intercalation after 2000 cycles. 124

Figure 5-6: (a) Optical absorption spectra of hierarchically porous MoO₃-MWCNTs composite with various weight ratios of MWCNTs compared MoO₃ nanowires. (b) Photocatalytic properties of hierarchically porous MoO₃-MWCNTs composites compared with MoO₃ nanowires. The TBO normalization concentration in the... 128

Figure 5-7: (a) the mineralization rate of contaminant was determined by measuring the disappearance of Total organic carbon (TOC) during the photocatalytic degradation of TBO by photocatalysis with hierarchically porous MoO₃-MWCNTs composite under visible light irradiation (λ〉 420 nm). (b) Dependence of the stability... 129

초록보기

Transition metal oxide one dimensional (1D) nanostructures are of great interest for the energy related devices because of their unique physical and chemical properties. The key limitation of the existing materials for energy storage is in the limited energy and power density. Hence, there is a considerable interest in exploring new materials which offer increased levels of energy storage. In this dissertation, transition metal oxide molybdenum oxide (MoO₃) and its composites with MWCNTs were synthesized via chemical solution routes. Structural and morphological studies were analyzed for the potential applications in photocatalysis, energy storage and conversion devices. The results indicate that low cost, environmental friendly nature and excellent capacitive properties of the MoO₃and MoO₃-MWCNTs nanocomposites lead to new photocatalytic applications and offer increased energy density while still maintaining their high-power-density.

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