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研究生(外文):Kevin Indrawan Sucipto
論文名稱:利用改變起始粉末晶面取向抑制 SrTiO3 第二相生成之研究
論文名稱(外文):Inhibition of second phase of interconnector by controlling surface orientation of SrTiO3 starting powder
指導教授(外文):Shao-Ju Shih
口試委員(外文):chen-hao wangChin-Yang YuYu-Jen Chou
外文關鍵詞:powders: chemical preparationelectron microscopyperovskites
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研究中分別於前驅物中添加三個不同濃度 (0.03, 0.15, 和0.45M)的雙氧水,並利用噴霧熱裂解法製備鈦酸鍶粉末,再於1500ºC下進行燒結1小時、1000ºC下退火24小時,最後與未添加雙氧水的試片進行比較。
最後由實驗結果得知,添加過氧化氫的多晶SrTiO3在1000℃ 24小時的熱處理下可以減少RP第二相的偏析。
Strontium titanate (SrTiO3)-based solid oxide fuel cell interconnectors have attracted more attention due to their chemical and physical stabilities. However, there is a phase segregation after become bulk specimen and annealed for period of time in high temperature. Second phase appeared on the Sr-rich (100) surface plane due to thermal decomposition of SrCO3. By controlling the crystalline SrTiO3 surface energy using hydrogen peroxide (H2O2), it can be lowering the {100} plane surface energy, so the population of {100} will be decreased. In this experiment, SrTiO3 powders were prepared by spray pyrolysis method using different concentration of H2O2 (0.03, 0.15, and 0.45M) and were sintered at 1500ºC for 1h and annealed at 1000ºC for 24h while comparing with un-treated sample. Spray pyrolysis was chosen because it is simple and able for continuous operation with high and uniform particles distribution result. As characterization, X-ray diffraction (XRD), Raman spectroscopy, and scanning electron microscopy (SEM) were conducted to research crystallographic phase and particle surface morphology. For bulk specimens, XRD, SEM-energy dispersive spectroscopy (EDS), Archimedes method, were conducted to research crystallographic phase, surface morphology, and relative density. Finally, H2O2-treated SrTiO3 bulk able to reduce the segregation of Ruddlesden Popper phase at 1000ºC for 24h.
摘要 II
Chapter 1. Introduction 1
1.1 Ceramic material 1
1.2 Strontium titanate second phase segregation 3
1.3 Purposes of this study 4
Chapter 2. Literature review 6
2.1 Solid Oxide Fuel Cell 6
2.1.1 Solid Oxide Fuel Cell Interconnector part 8
2.2 Interconnector material 10
2.3 Properties of strontium titanate 11
2.3.1 Crystal structure of strontium titanate 12
2.3.2 Physical properties of strontium titanate 13
2.3.3 Surface energy of strontium titanate 13
2.4 Phase composition of strontium titanate 14
2.4.1 Ruddlesden-Popper (RP) phases 15
2.4.2 RP phase formation 16
2.5 Sintering 17
2.5.1 Stages of sintering 18
2.5.2 Sintering method 21
2.6 Spray pyrolysis 22
2.6.1 Ultrasonic spray pyrolysis equipment 22
2.6.2 Particle formation in the spray pyrolysis method 25
Chapter 3. Experimental Procedure 28
3.1 Experimental materials 28
3.2 Experimental equipment 29
3.3 Preparation 31
3.3.1 Spray pyrolysis procedure 33
3.3.2 Die pressing and sintering 34
3.3.3 Annealing 34
3.4 Characterizations 35
3.4.1 X-ray diffraction 35
3.4.2 Nitrogen Adsorption/Desorption 35
3.4.3 Raman Spectroscopy 36
3.4.4 Field Emission Scanning Electron Microscope 37
3.4.5 Back-Scattered Electron Detector 39
3.4.6 Energy-dispersive X-ray Spectroscopy 40
3.4.7 Relative density 40
Chapter 4. Results 42
4.1 SrTiO3 powders 42
4.1.1 Crystallographic phase 42
4.1.2 SrTiO3 powder particle surface morphology 44
4.1.3 Surface area 47
4.2 SrTiO3 bulk after sintering process 48
4.2.1 Crystallographic phase 48
4.2.2 Cross sectional micrograph 50
4.2.3 Relative density 52
4.3 SrTiO3 bulk after sintering and annealing process 53
4.3.1 Crystallographic phase 53
4.3.2 Scanning electron micrograph 55
4.3.3 Cross sectional micrograph 60
4.3.4 Relative density 62
Chapter 5. Discussion 64
5.1 Influence of H2O2 to SrTiO3 particle shape 64
5.2 Influence of H2O2 to surface population. 65
5.3 SrTiO3 phase segregation 67
5.4 SrTiO3 bulk specimens’ grain 69
Chapter 6. Conclusions 73
Chapter 7. Future works 75
References 76
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