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Title Page
Contents
I. INTRODUCTION 11
I-1. Background and Purpose 11
I-2. Conducting Polymers 15
I-3. Structures and Conductivity of Conducting Polymers 17
I-4. Direct Methanol Fuel cell (DMFC) 21
I-5. Analytical Electrochemistry 23
I-5-1. Electrolytic System 23
I-5-2. Cyclic Voltammetry (CV) 27
I-5-3. Reversible, Irreversible and Quasi-reversible System 30
I-5-4. Chronoamperometry (CA) 32
I-5-5. Electrochemical Quartz Crystal Microbalance (EQCM) 34
II. EXPERIMENTAL 36
II-1. Introduction 36
II-2. Apparatus and Chemicals 38
II-3. Electrochemical Preparation of Polyaniline(PANi) 40
II-4. Cyclic Voltammogram and UV/Vis Spectra of PANi Films 42
II-5. Preparation of Conducting Polymer / Metal Composites 45
II-5-1. Preparation of Composites by Spontaneous Redox Reaction 45
II-5-2. Preparation of Composites by Electrochemical methods 47
II-6. Oxidation of Methanol on Composite electrodes 49
II-7. Quantitative Analysis 50
II-7-1. EQCM Proportionality Constant Calibration 50
II-7-2. Quantitative Aspect for Preparation and Characterization of PANi 51
II-7-3. Pt Loading 52
III. Results and Discussion 53
III-1. Preparation of PANi film 53
III-2. Characterization of PANi by in-situ UV/Vis Spectroelectrochemistry 55
III-3. Preparation of Conducting Polymer/Metal Composites 59
III-3-1. Preparation of Composites by Spontaneous Redox Reaction 59
III-3-2. Preparation of Composites by Electrochemical methods 63
III-4. Methanol Oxidation 71
III-5. Quantitative Analysis 76
III-5-1. EQCM Proportionality Constant Calibration 76
III-5-2. Quantitative Aspect for Preparation of PANi 81
III-5-3. Quantitative Aspect for Characterization of PANi 83
III-5-4. Pt Loading 86
IV. CONCLUSIONS 90
V. REFERENCES 91
Abstract 93
Table 1. Chemicals used in this study 39
Table 2. experimental conditions of aniline electropolymerization 40
Table 3. Experimental conditions for PANi characterization measurement 43
Table 4. experimental conditions for PANi reduction 45
Table 5. experimental conditions for Pt particles deposition by applying CA 47
Table 6. experimental conditions for Pt particles deposition by applying CV 48
Table 7. experimental conditions for methanol oxidation on composite electrodes 49
Table 8. experimental conditions of PANi preparation 51
Table 9. experimental conditions of PANi characterization 52
Table 10. The statistics of results of EQCM Proportionality Constant Calibration 77
Table 11. Platinum loading and methanol oxidation peak current density... 87
Figure1. Conducting polymers and their electrical conductivities 12
Figure2. Conductivity of some conducting polymers and other materials 16
Figure3. Energy level of π molecular orbital for polyacetylene 19
Figure4. Evolution of midgap states in polypyrrole upon doping 20
Figure5. A schematic of the operating principles a Direct Methanol Fuel Cell 22
Figure6. Schematic diagram of electrolytic system 25
Figure7. Equivalent circuit for potentiostate based on feedback circuit 26
Figure8. Cyclic voltammetric excitation signal 29
Figure9. Cyclic voltammogram for a freely diffusing species 29
Figure10. CV for reversible process (the scan rate a: 1, b: 10, c: 50, d: 100V/sec) 31
Figure11. CV for irreversible process (the scan rate a: 1, b: 10, c: 50, d: 100V/sec) 31
Figure12. The potential-time profile for a single potential step chronoamperometry 33
Figure13. Current-time responses for a potential step experiment. E₂ was chosen so... 33
Figure14. Schematic diagram of EQCM electrode and electrolytic system 35
Figure15. The mechanism of aniline electropolymerizaiton 41
Figure16. Electrodes configuration in UV/Vis cell for spectroelectrochemical... 44
Figure17. Electrochemical synthesis of PANi: (a) CV of aniline polymerization and... 54
Figure18. Specroelectrochemical properties of PANi: CV (a), in-situ UV/Vis... 57
Figure19. (a)CV of PANi at the potential range of -0.1V~0.6V, (b) SEM images of... 58
Figure20. Reduction process of PANi: (a) current-time curve and (b) in-situ... 60
Figure21. UV/Vis spectra changes during PANi/Pt composite formation: (a) UV/Vis... 62
Figure22. Cyclic voltammogram during the Pt particles formation and... 65
Figure23. CA curves of Pt deposited at the constant potential of (a) -0.25 v(b)-0.35 v... 66
Figure24. SEM images and EDAX spectrum of PANi/Pt composite electrodes: (a)... 70
Figure25. CVs of methanol oxidation (a) on PANi electrode, (b) on pure Pt electrode;... 75
Figure26. I-t figure and frequency change during the deposition process at the... 80
Figure27. Cyclic voltammogram (a) and in-situ monitoring of frequency... 82
Figure28. Cyclic voltammogram (a) and in-situ monitoring of frequency change (b)... 84
Figure29. The frequency change concurrently recorded with cyclic voltammograms... 85
Figure30. Frequency change as a function of time during the process of Pt doping... 89
초록보기 더보기
Polyaniline(PAni)은 특히 친환경적 안정성과 넓은 범위의 전도성, 서로 다른 산화/환원상태가 존재한다. 몇몇 금속의 소립자는 유기 화합물에 좋은 촉매 활성도를 보여준다.
본 연구에서는 고분자/금속화합물의 전도성 특성과 제조과정에 중점을 두었다. PANi 은 전기 화학적 고분자로 제조된다. Pt 입자들은 PANi 필름에서 두 가지 방법으로 분산된다.
일정 또는 순환전압에 의해 전기화학적 형성과 환원된 PANi 과 PtC162-에서 자발적인 환원반응에 의한 것이다. 고분자 형성과정과 Pt 증착은 EQCM 으로 정량적 측정이 가능하다. PANi/Pt 전극에서 메탄올의 촉매 분해는 순환전압법을 이용함으로써 측정할 수 있다.
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