以常壓電漿噴射束製備奈米陶瓷粉體之微觀特性、化性及電性研究

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研究生：	蘇昱銘 Yu-Ming Su
論文名稱：	以常壓電漿噴射束製備奈米陶瓷粉體之微觀特性、化性及電性研究 Microstructure Characterization, Chemical Stability, and Electrical Property of Ceramics Nanopowders Synthesized by Atmospheric Pressure Plasma Jet
指導教授：	郭俞麟 Yu-Lin Kuo
口試委員:	韋文誠 Wen-Cheng J. Wei 張宏宜 Horng-Yi Chang 楊永欽 Yung-Chin Yang 洪逸明 Hung I-Ming 施劭儒 Shao-Ju Shih 周宏隆 Hung-Lung Chou 江偉宏 Wei-Hung Chiang
學位類別：	博士 Doctor
系所名稱：	工程學院 - 機械工程系 Department of Mechanical Engineering
論文出版年：	2014
畢業學年度：	102
語文別：	英文
論文頁數：	151
中文關鍵詞：	固態氧化物燃料電池、氧化釓掺雜氧化鈰、密度泛函理論、奈米顆粒
外文關鍵詞：	Solid Oxide Fuel Cells, Gd2O3-doped CeO2, Density functional theory, Nanoparticles
相關次數：	點閱：368 下載：0
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本研究利用常壓噴射束電漿(Atmospheric pressure plasma jet, APPJ)製備氧化釓掺雜氧化鈰（Gd2O3-doped CeO2, GDC）奈米顆粒，並以硝酸鈰與硝酸釓混合溶液作為前驅物製備來源。主要探討不同Gd摻雜濃度對於GDC奈米顆粒其結晶性質、表面型態、微觀結構及電性能之影響。製備後之粉體材料性質分析分別以X光繞射儀(XRD)分析其結晶結構及粉體尺寸，掃描式電子顯微鏡(SEM)與穿透式電子顯微鏡(TEM)觀察其表面形貌與粉體尺寸，最後以電漿放射光譜分析(OES)進一步研究其氧化物顆粒成型之機制，結果顯示經由常壓電漿噴射束能於短時間內製備出GDC立方相螢石結構之奈米粉體。
實驗及理論分析於三價金屬離子摻雜氧化鈰基材料之研究已受到許多關注，因其可應用於固態氧化物燃料電池之電解質材料。第一原理密度泛函理論（DFT）研究能提供詳細的原子級結構分析及改善電解質材料之問題，並有助於了解GDC奈米結構之應用。本研究利用密度函數理論模擬CeO2、Ce0.9Gd0.1O2的電荷分佈。藉由CeO2和Ce0.9Gd0.1O2的Bader charge分析之結果，顯示以Gd作為摻雜物有助於增加Ce0.9Gd0.1O2奈米結構之電荷，提升Ce0.9Gd0.1O2之導電性能。

Gd2O3-doped CeO2 (GDC) nanoparticles were prepared thought a facile one-step fabrication from a precursor solution via atmospheric pressure plasma jet (APPJ). The mixture precursor solution of gadolinium nitrate hexahydrate and cerous nitrate hexahydrate were used as initial precursors for Gd and Ce ions. The microstructure of GDC was found to be an assembly of nanocrystallites with a cubic fluorite structure analyzed by XRD and TEM. Reactive oxygen species (detected by optical mission spectroscopy (OES)) are believed to be the major oxidative agents for the formation of oxide materials in the APPJ process. Based on the materials characterization and OES observations, the proposed formation mechanism of GDC nanoparticles by APPJ was illustrated in this study. The results of the study effectively demonstrated the feasibility of preparing well-crystallized GDC nanoparticles by the APPJ system.
Theoretical and experimental studies based on trivalent metal ions doped-ceria have received major attention due to its possible applications as the electrolyte material within solid oxide fuel cells (SOFCs). First principles density functional theory (DFT) study of ceria-based materials can provide a detailed understanding of the atomic level properties and contribute towards the hunt for improved electrolyte material. A better understanding of this interaction will facilitate the design of better conjugates for Ce0.9Gd0.1O2 nanocrystals for various applications. The detailed mechanism is not clear until now. In this study, the density function theory (DFT) simulation was employed to demonstrate charge analyses of CeO2 and Ce0.9Gd0.1O2. By comparing the Bader charge of the bare CeO2 and Ce0.9Gd0.1O2 nanocrystals, it was shown that Gd as doped metal help to increase the charge on Ce0.9Gd0.1O2 nanocrystals.

Table of contents
摘要	..I
Abstract	.II
Acknowledgements	...V
Table of contents	IV
List of figures	VIII
List of tables	.XII
Chapter 1 Introduction
1.1 Motivation	1
1.2 Objective of the research	3
Chapter 2 Literature review
2.1 Introduction of SOFCs	5
2.2 Working principles of SOFCs	8
2.3 Solid Electrolyte for SOFCs	8
2.3.1 Perovskite-Structured Solid State Electrolytes	9
2.3.2 La2Mo2O9 (LAMOX) Electrolyte	13
2.3.3 Apatite-Structured Solid State Electrolytes	14
2.3.4 Fluorite-Structured Solid State Electrolytes	17
2.3.4.1 Bismuth Oxide-based Electrolyte	17
2.3.4.2 Zirconia-Based Electrolytes	18
2.3.4.3 Ceria-Based Electrolytes	20
2.3.5 Fabrication of Ceria-Based Electrolyte Material	25
2.3.5.1 Solid State Reaction Method	25
2.3.5.2 Sol-Gel Method	26
2.3.5.3 Glycine-Nitrate Combustion Process (GNP)	27
2.3.5.4 Spray Pyrolysis	29
2.3.6 Atmospheric Pressure Plasma Fabrication for the production of SOFC components	30
2.3.6.1 Plasmas classification	31
2.3.6.2 Atmospheric Pressure Plasmas: LTE or non-LTE	32
2.3.6.3 Thermal Plasma Spray	37
2.3.6.4 Cold atmospheric plasma sources (Non-equilibrium Plasmas)	39
Chapter 3 Experimental Set-Up
3.1 Experimental Procedures	43
3.2 Materials Characterization of Prepared Samples	44
3.2.1 Measurement of Plasma Temperature	42
3.2.2 Optical Emission Spectroscopy	42
3.2.3 X-Ray Diffraction Analysis & Rietveld Analysis	42
3.2.4 Field Emission Scanning Electron Microscopy	43
3.2.5 High Resolution Transmission Electron Microscopy	43
3.2.6 X-ray Photoelectron Spectroscopy	43
3.2.7 Laser Diffraction for Particle Size Distribution	45
3.2.8 TGA Analysis of Prepared Samples	46
3.2.9 AC Impedance	46
3.3 Computation Details	46
Chapter 4 Material Characterization of Gd2O3-doped CeO2
4.1 Basic Plasma Characterization	48
4.2 Preparation of ZrO2 particle	51
4.3 Preparation of Gd2O3 doped-CeO2particles	66
4.3.1 TGA Analysis of Prepared Samples	66
4.3.2 X-ray Diffraction and Rietveld Refinement Analysis	69
4.3.3 TEM Analysis	72
4.3.4 DFT calculation and Bader charge analyses	73
Chapter 5 Chemical Stability and Electrical Performance of Gd2O3-doped CeO2
5.1 Background	..95
5.2 Thermal Stability of Gd2O3-doped CeO2	..98
5.3 Electrical Performance of Gd2O3-doped CeO2	107
Chapter 6 Conclusions	115
Reference	116
 
List of Figures
Figure 2.1 Working principle of SOFCs	7
Figure 2.2 Examples of compounds showing (a) order-disorder transitions and (b) their doped counterparts. Data are taken from: Bi2O3 [39], Bi4V2O11 [40], Ba2In2O5 [23], La2Mo2O7 [41], 0.8Bi2O3•0.2Er2O3 [42], Bi4V1.8Cu0.2O10.7 [40], (Ba0.3Sr0.2La0.5)2In2O5 [28], and La1.8Gd0.2Mo1.8W0.2O7 [43]	11
Figure 2.3 Conductivity data for YSZ [44], CGO [45], and LSGM [35]	11
Figure 2.4 Representation of the structure of apatite viewed down the c axis; the XO4 tetrahedra are yellow, the lanthanum and oxygen atoms are gray and red spheres	15
Figure 2.5 Ionic conductivity of ZrO2-Y2O3 solid solutions at 300 °C. Reproduced with permission from ref [45]	18
Figure 2.6 Results for a CGO electrolyte supported (0.8 mm thick) solid oxide fuel cell with 97 vol % H2 + 3 vol%H2O, Ni-CGO anode/CGO electrolyte/PBCO-CGO cathode, air from 500 to 700 °C at 25°Cintervals. The inset is the temperature dependence of the open circuit voltage	21
Figure 2.7 Sol-Gel technologies and their products	24
Figure 2.8 General schematic of a spray pyrolysis deposition process.	26
Figure 2.9 Evolution of the plasma temperature (electrons and heavy particles) with the pressure in a mercury plasma arc	32
Figure 2.10 Principle of a corona discharg	37
Figure 2.11 Principle of dielectric barrier discharge	38
Figure 3.1 APPJ system	41
Figure 4.1 Plasma Temperature at 300, 400, and 500.	48
Figure 4.2 Optical emission spectrum of the CDA plasma with atomized precursors and O2 carrier gas	48
Figure 4.3 FESEM photographs of the prepared zirconia particles: (a) 300 W, (b) 400 W, and (c) 500 W	58
Figure 4.4 Particle size distributions of prepared zirconia particles: (a) 300 W, (b) 400 W, and (c) 500 W.	59
Figure 4.5 XRD spectra of prepared zirconia particles at 300, 400, and 500W	60
Figure 4.6 XPS spectra of (a) Zr 3d, and (b) O 1s core levels for the prepared zirconia particles.	61
Figure 4.7 (a) TEM image, (b) SAED pattern, and (c) TEM-EDS pattern, of prepared zirconia particles for 400	62
Figure 4.8 Proposed mechanism for the formation of prepared zirconia particles from atomized solution droplets in an APPJ process	63
Figure 4.9 The TGA analysis results of (a) weight loss and (b) differential versus temperature for Ce(NO3)3．6H2O precursor	75
Figure 4.10 The TGA analysis results of (c) weight loss and (d) differential versus temperature for Gd(NO3)3．6H2O precursor	76
Figure 4.11 XRD spectra and Rietveld refinement analysis of prepared (a) CeO2, (b) 10GDC, and (c) 20GDC by APPJ	78
Figure 4.12 HR-TEM images, FFT pattern and particle size distribution of prepared (a, c) CeO2 and (b, d) 10GDC nanoparticles by APPJ	79
Figure 4.13 HR-TEM images of prepared 10GDC nanoparticles	80
Figure 4.14 TEM image and elemental mapping images of 10GDC nanoparticles	81
Figure 4.15 HR-TEM images of prepared 20GDC nanoparticles	82
Figure 4.16 TEM image and elemental mapping images of 20GDC nanoparticles	83
Figure 4.17 HR-TEM images of prepared 40GDC nanoparticles	84
Figure 4.18 TEM image and elemental mapping images of 4GDC nanoparticles	85
Figure 4.19 The model of top-view of CeO2 (111)	86
Figure 4.20 The model of alternative-view of CeO2 (111)	87
Figure 4.21 The model of side-view of CeO2 (111)	88
Figure 4.22 The model of side-view of CeO2 (111)	89
Figure 4.23 The model of top-view of Gd (001)	90
Figure 4.24 The model of alternative-view of Gd (001)	91
Figure 4.25 The model of side-view of Gd (001)	92
Figure 4.26 The model of side-view of Gd (001)	93
Figure 4.27 The model of top-view of Ce0.9Gd0.1O2 (111)	94
Figure 4.28 The model of alternative-view of Ce0.9Gd0.1O2 (111)	95
Figure 4.29 The model of side-view of Ce0.9Gd0.1O2 (111)	96
Figure 4.30 The model of side-view of Ce0.9Gd0.1O2 (111)	97
Figure 4.31 The model of top-view of Ce0.8Gd0.2O2 (111)	98
Figure 4.32 The model of alternative-view of Ce0.8Gd0.2O2 (111)	99
Figure 4.33 The model of side-view of Ce0.8Gd0.2O2 (111)	100
Figure 4.34 The model of side-view of Ce0.8Gd0.2O2 (111)	101
Figure 5.1 Isothermal Reduction of (a) CeO2, (b)10GDC, and (c) 20GDC	109
Figure 5.2 Activation Energy of (a) CeO2, (b)10GDC, and (c) 20GDC	110
Figure 5.3 XRD analysis of reduced (a) CeO2, (b)10GDC, and (c) 20GDC	111
Figure 5.4 TEM images of (a) 10GDC and (b) 20GDC by APPJ process, and (c) 10GDC by sol-gel method	112
Figure 5.5 SEM images of (a) 10GDC and (b) 20GDC by APPJ process, sintered at 1300 °C	113
Figure 5.6 SEM images of (a) 10GDC and (b) 20GDC by APPJ process, sintered at 1400 °C	114
Figure 5.7 SEM images of (a) 10GDC and (b) 20GDC by APPJ process, sintered at 1500 °C	115
Figure 5.8 AC impedance of all samples sintered at 1400°C and measured at (a) 800, (b) 700, (c) 600, (d) 500, and (e) 400 °C	118
Figure 5.9 AC impedance of all samples sintered at 1500 °C and measured at (a) 800, (b) 700, (c) 600, (d) 500, and (e) 400 °C	121
Figure 5.9 AC impedance of all samples sintered at 1500 °C and measured at (a) 800, (b) 700, (c) 600, (d) 500, and (e) 400 °C	121
Figure 5.9 AC impedance of all samples sintered at 1500 °C and measured at (a) 800, (b) 700, (c) 600, (d) 500, and (e) 400 °C	121

List of Tables
Table 2-1 Conductivity of Some Lanthanum Silicate Apatites (data from ref 54)	15
Table 2-2 Some physical properties of pure stoichiometric CeO2	21

                                

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