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研究生:陳福強
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:施劭儒
指導教授(外文):Shao-Ju Shih
口試委員:王丞浩游進陽周育任
口試委員(外文):chen-hao wangChin-Yang YuYu-Jen Chou
口試日期:2019-01-07
學位類別:碩士
校院名稱:國立臺灣科技大學
系所名稱:材料科學與工程系
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2019
畢業學年度:107
語文別:英文
論文頁數:100
中文關鍵詞:粉末化學製備法電子顯微鏡鈣鈦礦
外文關鍵詞:powders: chemical preparationelectron microscopyperovskites
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以鈦酸鍶作為固態氧化物燃料電池連接板之研究倍受關注,因其具有良好的化學及物理穩定性。然而,高溫退火處理形成之多晶樣品會發生相分離現象。第二相出現在具有較高鍶濃度的(100)平面,其源自於碳酸鍶的熱分解作用。
本研究之目的希望利用過氧化氫來控制SrTiO3¬晶體的表面能,達到降低{111}面族表面能,進而使{100}晶面減少。
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。
選擇使用噴霧熱裂解法製備是因為它簡單且能夠連續操作,具有高均勻的顆粒分佈結果。本研究合成之粉體部分利用X光繞射分析儀(XRD)、拉曼光譜儀、掃描式電子顯微鏡(SEM)、氮氣吸脫附分析儀(BET)分別鑒定相組成、表面形貌及比表面積。而燒結體則使用能量色散X-射線光譜(EDS)、XRD、阿基米德法分別進行相組成、表面形貌(元素組成)、相對密度。
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.
CONTENTS
摘要 II
ABSTRACT V
ACKNOWLEDGEMENTS VI
CONTENTS VII
LIST OF FIGURES XI
LIST OF TABLES XV
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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