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Title Page
Abstract
국문요약
Contents
Chapter 1. Introduction 13
1-1. Research background 13
1-2. Objective of the thesis 15
Chapter 2. Anodic Alumina Oxide (AAO) 17
2-1. Introduction 17
2-2. Pore formation mechanism 18
2-3. Experimental details 21
2-3-1. Preparation of Al for Anodization 21
2-3-2. Anodization of Aluminum 23
2-3-3. Preparation of free-standing AAO 26
2-3-4. Fabrication of AAO on Si substrate 27
2-4. Results and Discussion 28
2-4-1. Electropolishing effect on anodization 28
2-4-2. The second anodization effect on pore arrangement in AAO 30
2-4-3. Fabrication of free-standing nanoporous alumina film 34
2-4-4. Pore wall etching (Pore widening) 36
2-4-5. AAO in Si wafer 39
2-5. Summary for chapter 2 43
Chapter 3. Fabrication of Macroporous Si 44
3-1. Introduction 44
3-2. Chemical dissolution of Si 45
3-3. Experimental details 48
3-3-1. Experimental setup and important parameters 48
3-3-2. I-V measurements 50
3-3-3. Sample preparation 52
3-3-3-1. For disordered macroporous Si 52
3-3-3-2. For ordered macropore arrays 52
3-3-4. Photoelectrochemical etching of n-type Si 55
3-3-4-1. Disordered macropore arrays 55
3-3-4-2. Ordered macropore arrays by 55
3-4. Results and Discussions 57
3-4-1. I-V characterizations 57
3-4-2. Disordered macroporus Si array 60
3-4-3. Ordered macroporous Si arrays 63
3-5. Summary for the chapter 3 68
Chapter 4. Ferroelectric Lead Zirconate Titanate (PZT) nanotubes by using template and MOD source 69
4-1. Introduction 69
4-1-1. Charactristics of ferroelectric materials 70
4-1-2. Characteristics of PZT 75
4-1-3. Basics of wetting process 77
4-2. Experimental section 81
4-2-1. Contact angle measurement 81
4-2-2. Preparation of PZT nano-microtubes 83
4-3. Results and discussions 85
4-3-1. PZT nanotubes using AAO templates 85
4-3-2. PZT microtubes using macroporous Si template 87
4-3-3. XRD characterization of PZT nanotubes 89
4-3-4. TEM characterizations of PZT nanotubes 90
4-4. Summary for the chapter 4 92
Chapter 5. Pt Electrode Nanotubes 93
5-1. Introduction 93
5-2. Experimental details 93
5-3. Results and discussion 94
5-3-1. FE-SEM characterization of Pt nanotubes 94
5-3-2. XRD and TEM characterizations of Pt nanotubes 95
5-4. Summary for the chapter 5 97
6. Summary 98
7. Future works 99
Reference 100
Acknowledgements 105
[Figure 2-1] Schematic diagram of current density curve during anodization 20
[Figure 2-2] Schematic illustration of the pore formation at the beginning of the anodization 20
[Figure 2-3] Experimental set-up for anodization process 25
[Figure 2-4] Schematic illustration free standing AAO template preparation process 26
[Figure 2-5] Electropolishing effect on pore formation during anodization process 29
[Figure 2-6] Effect of two-step anodization on pore arrangement in AAO 33
[Figure 2-7] Free-standing AAO film obtained by chemically etching of the Al substrate 35
[Figure 2-8] Schematic representation of the AAO structure showing inner and outer oxide layers 37
[Figure 2-9] Pore wall etching effect on AAO morphology 38
[Figure 2-10] FE-SEM images of AAO on Si substrate, obtained by two-step anodization in sulfuric acid 41
[Figure 2-11] Anodic alumina on Si substrate obtained after first step anodization in 0.3 M oxalic acid, at 40 V 42
[Figure 2-12] I-t characteristics for anodization process using Si based Al film 42
[Figure 3-1] Divalent chemical dissolution reaction of silicon in an HF solution 47
[Figure 3-2] Experimental set-up for photoelectrochemical etching of Si 49
[Figure 3-3] I-V curve for electrochemical etching of n-type Si in HF solution 51
[Figure 3-4] Process flow to prepare Si sample for electrochemical etching process by photolithography 54
[Figure 3-5] I-V characteristics of n-type Si for 5 wt. % 58
[Figure 3-6] SEM images of the electrochemicaly etched Si during I-V characterization 59
[Figure 3-7] Disordered macroporous Si obtained by photoelectrochemical etching method 62
[Figure 3-8] Dependence of current density on average pore diameter 63
[Figure 3-9] OM image of patterned Si wafer 65
[Figure 3-10] SEM images of Si wafer after KOH etching through SiO₂ mask 66
[Figure 3-11] SEM image of ordered macroporous Si arrays etched in patterned n-type Si 67
[Figure 4-1] ABO₃ perovskite unit cell 71
[Figure 4-2] Typical polarization hysterisis loop of a ferroelectric capacitor 74
[Figure 4-3] Phase diagram of PZT 76
[Figure 4-4] Illustration of dependence between wetting stages and contact angle 78
[Figure 4-5] Transition of a liquid wedge by an amount dx 78
[Figure 4-6] Contact angle variation by polymer source ratio in PZT solution 82
[Figure 4-7] Flow chart for the template wetting process 84
[Figure 4-8] FE-SEM images of the PZT microtubes obtained by using AAO template 86
[Figure 4-9] SEM images of the vertically aligned PZT microtubes obtained by using macroporous Si template 88
[Figure 4-10] XRD patterns of the PZT nanotubes 90
[Figure 4-11] TEM and SAED images of the PZT nanotubes 91
[Figure 5-1] FE-SEM image of Pt nanotubes obtained by baking at 200 °C for 24 h and annealed at 300℃ for 1 h 94
[Figure 5-2] XRD patterns of Pt nanotube 96
[Figure 5-3] TEM images of Pt nanotube 96
[Table 2-1] Anodization conditions to prepare ordered nanopore array 24
[Table 2-2] Experimental conditions for anodization of Al/Si substrate 40
[Table 4-1] Summarized PZT ? Polymer I mixture ratios used in contact angle measurement experiment 81
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