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研究生:LE MINH VIEN
研究生(外文):LE MINH VIEN
論文名稱:Cerium pyrophosphate for proton exchange membrane fuel cell at intermediate temperature
論文名稱(外文):Cerium pyrophosphate for proton exchange membrane fuel cell at intermediate temperature
指導教授:蔡大翔
指導教授(外文):Dah-Shyang Tsai
口試委員:蔡大翔
口試日期:2011-07-05
學位類別:博士
校院名稱:國立臺灣科技大學
系所名稱:化學工程系
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2011
畢業學年度:99
語文別:英文
論文頁數:122
外文關鍵詞:Cerium pyrophosphatecerium diphosphateintermediate temperature fuel cellMg-doped cerium pyrophosphateproton exchange membrane fuel cell
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摘要
藉由磷酸將氧化鈰溶解製備出摻雜與未摻雜焦磷酸鈰。本研究將探討其質子導電率與水分影響並應用於中溫層的質子交換膜燃料電池的發展性。
在起始鈰與磷的比例為1比2~2.4間,在300與450oC下一純相的CeP2O7的鈰與磷的比例約為1比2.3,而在較高的溫度下合成時會導致其他雜相生成,其裂解溫度在750oC以上。CeP2O7的結晶結構可是為一擬立方晶相,但實際上為三斜晶。在300、450、600、750與900oC燒結的CeP2O7以450oC擁有較高的質子導電率,其在120~180oC間,通入濕空氣(其水分壓為0.114 atm)時所測得質子導電率皆超過0.01 Scm-1,且於180oC時測得3x10-2 Scm-1。藉由傅立葉紅外線光譜儀(FT-IR)確認燒結450oC時粉末的吸濕性比燒結300oC時粉末高。以厚度0.5mm CeP2O7電解質所製備之電池,在200oC下通入50 %H2與空氣時,擁有電功率密度為22 mWcm-2。
在鈰的位置摻雜鎂不僅可以提升其導電性且使得其工作溫度範圍變得寬。藉由傅立葉紅外線光譜儀(FT-IR)發現鎂摻雜焦磷酸鈰比未摻雜焦磷酸鈰擁有更佳的保濕性並由熱重分析儀(TGA)確認以10 mol%鎂摻雜的焦磷酸鈰比未摻雜焦磷酸鈰在濕空氣中可以吸收更多的水分。
在電性量測分面,以10 mol%鎂摻雜焦磷酸鈰電解質所製備之電池,在操作溫度140~260oC間,通入50 %H2濕空氣(其水分壓為0.114 atm)量測,以0.36mm厚度的電解質與其搭配陰陽極為CMP : Pt/C : PTFE (42.5: 42.5:15)在240oC時擁有較佳電功率密度表現達40 mWcm-2且開環電壓為0.65 V。
ABSTRACT

Doped and un-doped cerium pyrophosphates have been prepared via phosphoric acid digestion of cerium oxide. Their proton conductivities and water affinities are studied with the aim of developing a proton exchange membrane fuel cell at intermediate temperatures.
Among the starting Ce:P ratios between 1:2.0 and 1:2.4, a pure CeP2O7 phase is prepared with the 1:2.3 ratio at 300 and 450oC. Higher synthesis temperatures lead to impurity phases. Extensive decomposition occurs at temperature above 750oC. Crystal structure of CeP2O7 may be described using a pseudo-cubic cell, but more precisely a triclinic cell. The 450oC-sintered CeP2O7 disk exhibits a higher proton conductivity, compared with 300, 600, 750, 900oC-sintered specimens. The proton conductivity of CeP2O7 is more than 0.01 S cm-1 between 120 and 180oC in moist air of water partial pressure PH2O=0.114atm, with a maximum value of 3.0?e10-2 S cm-1 at 180oC. The conductivity depends on humidity and operating temperature. FT-IR results confirm that 450oC-sintered powder is more hygroscopic than 300oC-sintered powder. A fuel cell using 0.5 mm thick CeP2O7 electrolyte is evaluated used 50%H2 and air as fuel and oxidant. Its peak powder density is ??2 mW cm-2 at 200oC.
Partial substitution of Mg not only raises the conductivity, but also shifts and widens the relevant temperature window. FTIR results indicate that Ce0.9Mg0.1P2O7 is more capable in retaining water than CeP2O7. The TGA results confirm that the 10 mol% Mg-doped CeP2O7 can absorb more water from moist air than that of un-doped CeP2O7.

Performance of a fuel cell using Ce0.9Mg0.1P2O7 electrolyte is investigated in the temperature range of 140 - 260oC under humidified air PH2O=0.114 atm. The fuel cell generates power 40 mW cm-2 when consuming 50% hydrogen at 240oC and 0.65V, using 0.36 mm thick Ce0.9Mg0.1P2O7 and the catalyst ink with CMP:Pt/C:PTFE ratio of 42.5:42.5:15 for anode and cathode.
ABSTRACT i
ACKNOWLEDGEMENTS v
CONTENTS vii
LIST OF FIGURES x
LIST OF TABLES xiv
LIST OF TABLES xiv
LIST OF ABBREVIATIONS AND SYMBOLS xv
Chapter 1 Fuel cell as an efficient energy conversion device 1
1.1 Principle of fuel cells 1
1.1.1 Fuel cell thermodynamics and performance 3
1.1.1.1 Fuel cell efficiency: 3
1.1.1.2 Fuel cell performance: 4
1.1.2 Classification 6
1.2 Proton Exchange membrane fuel cells (PEMFCs) and components 9
1.2.1 Membrane 11
1.2.2 Catalyst layers 12
1.2.3 Gas diffusion layer (GDL) 13
1.2.4 Bipolar plate 14
1.3 Proton transport mechanism and proton conducting materials 14
1.3.1 Proton conducting mechanism 14
1.3.2 Proton conducting materials: 16
1.3.2.1 Proton conduction mechanism in liquid state 16
1.3.2.2 Proton conduction mechanism in solid state 17
Chapter 2 Raising the temperature of exchange membrane fuel cell 25
2.1 Potential advantages of intermediate-temperature fuel cells 25
2.1.1 High CO tolerance: 25
2.1.2 Elimination of external humidification 26
2.1.3 Direct use of alternative fuels: 26
2.1.4 Reducing platinum catalyst loading or adopting non-platinum catalyst: 27
2.2 Potential disadvantages: 27
Aim and organization of this thesis 29
Chapter 3 Experimental details 31
3.1 Sample synthesis: 31
3.2 Sample characterization 32
3.2.1 X-Ray Diffraction 32
3.2.2 Rietveld refinement 32
3.2.3 Electron Microscope 36
3.2.4 Thermal gravimetric analysis 36
3.2.5 Infrared spectroscopy 36
3.2.6 Density measurements 36
3.2.7 Impedance Spectroscopy 37
3.2.8 Fuel cell characterization 38
Chapter 4 Results and discussion 41
4.1 CeP2O7 electrolyte 41
4.1.1 Crystal structure and phase analysis 41
4.1.2 Impedance spectra and proton conductivities of CeP2O7 50
4.1.3 Infrared analysis 58
4.1.4 TG analysis 60
4.1.5 Fuel cell performance using CeP2O7 electrolyte 61
4.2 Mg2+-doped CeP2O7 electrolyte 62
4.2.1 Phase study of Mg2+-doped CeP2O7 62
4.2.2 Impedance spectra and proton conductivities of Mg2+-doped CeP2O7 68
4.2.3 Proton conductivities of metal cations-doped CeP2O7 71
4.2.4 Infrared analysis 73
4.2.5 TG analysis 75
4.2.6 Fuel cell performance using Ce0.9Mg0.1P2O7 76
4.2.6.1 Influence of catalyst components on fuel cell performance 76
4.2.6.2 I-V, I-P characteristics and electrolyte thickness effect 79
4.3 Summary 82
Chapter 5 CONCLUSIONS 83
References 85
LIST OF PUBLISHED PAPERS 98
Curriculum Vitae 99
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