Design, Characterization, and Fabrication of Sulfur Nanocomposite Cathode Material for High Performance Lithium-Sulfur Batteries

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研究生：	Tilahun Awoke Zegeye Tilahun - Awoke Zegeye
論文名稱：	Design, Characterization, and Fabrication of Sulfur Nanocomposite Cathode Material for High Performance Lithium-Sulfur Batteries Design, Characterization, and Fabrication of Sulfur Nanocomposite Cathode Material for High Performance Lithium-Sulfur Batteries
指導教授：	郭中豐 Chung-Feng Kuo 黃炳照 Bing-Joe Hwang
口試委員:	蘇威年 Wei-Nien Su 黃昌群 Chang-Chiun Huang 鄭銘堯 Ming-Yao Cheng 陳景翔 Ching-Hsiang Chen
學位類別：	博士 Doctor
系所名稱：	工程學院 - 材料科學與工程系 Department of Materials Science and Engineering
論文出版年：	2017
畢業學年度：	105
語文別：	英文
論文頁數：	174
中文關鍵詞：	鋰硫電池、微孔碳、介孔C摻雜TiO2 、混合、石墨烯、高硫負載、循環穩定性、N-摻雜、溶液滴、多硫化物核殼
外文關鍵詞：	Lithium-sulfur battery, microporous carbon, mesoporous C-doped TiO2, hybrid, graphene, high sulfur loading, cycle stability, N-doping, solution drop, polysulfides core-shell
相關次數：	點閱：312 下載：3
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鋰-硫（Li-S）電池領域在過去幾十年中已進行大量研究，期望尋找能達成高容量、長循環壽命、安全性改進、高倍率性能和高硫負載等商業化目標之正極材料。雖然已有顯著的成就，但實際應用的問題尚未完全解決，本研究目標為開發可用於高性能Li-S電池之高效陰極材料設計。首先以摻雜二氧化鈦與硫之微孔、中孔碳的複合材料(MC-Meso C摻雜TiO2/S)作為Li-S電池的陰極材料。通過低成本的水熱法和退火程序製備混合MC-Meso C摻雜TiO2/S之主體材料。所得的導電材料具有多微孔與中孔特性，可增強了硫和多硫化物之有效結合。此複合材料成功將碳摻雜入TiO2奈米管結構中，並將硫以熔融態注入時，可均勻分佈在此複合材料中。混合陰極材料在電化學測量中也顯示具有高硫含量（61.04 wt％），可有效改善循環穩定性和性能。此外材料在0.1C速率下以初始電容量802 mAh g-1，於140次循環之後能保有578 mAh g-1 且庫侖效率大於97.1％。此原因乃是本複合材料之特殊的奈米混合結構，並可均勻將硫分散至多中空微孔之奈米管結構中。
其次，本研究設計了一新型硫浸漬方法，將高重量比之硫（80 wt％）嵌入摻雜氮的三維石墨氧化物（3D N-RGO）中以組成新型奈米複合陰極材料。相較於原始石墨烯，氮摻雜可增加十倍表面積和七倍孔體積。這些結構特徵允許陰極容納更多的硫。此外陰極可吸附多硫化物並防止它們從主體材料脫離，可達成穩定的循環性能。溶液滴硫浸漬法可使奈米硫分佈均勻。此外陰極以1042 mAhg-1和916 mAh g-1的高初始電容量，在100次循環後分別在0.2C和0.5C下仍電容量仍保持優異94.8％和81.9％，而在500次循環下的每個循環中依然保持0.062％的低衰減率。由前述可知，結合溶液滴硫浸漬法和參雜氮的組合可作為解決容量衰減以及長循環問題之有效手段，並且提供可增加硫負載之新策略。
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第三，我們提出具有雙限制之硫陰極核-殼結構之新型設計，其中硫（72.5 wt％）嵌入石墨烯（G）殼中並包封在MC芯中。較大的可溶性多硫化物中間體（Li2Sx，4≤x≤8）被G殼捕獲，以防止可溶性多硫化物中間體溶解至有機電解質中，得以實現穩定的循環性能。此外，G殼體內保有中空間，可確保混合式陰極在循環時抵抗體積膨脹並保持完整性；另一方面MC在其小孔內限制較小的硫（S2-4）分子以抑制可溶性多硫化物的形成。前述所得到的電極可提供982 mAh g-1的高初始放電容量，在0.2C速率下100次循環後具有85.4％的增強容量保持率。更重要的是，陰極表現出886 mAh g-1的高放電容量，並且在0.5C下500次循環後仍能保持在601 mAh g-1，庫侖效率接近100％，此為循環穩定性中之最佳性能。

In the field of lithium-sulfur (Li-S) battery, intense research has been made in the past decades to find high capacity, long cycle life, improved safety, high rate capability, and high sulfur loaded cathode material for Li-S batteries to be applicable for commercialization. Although significant achievements have been established, problems that hindered real applications of Li-S batteries have not been fully resolved. Therefore, this dissertation focused on the design of sulfur nanocomposite cathode material for high performance Li-S batteries and characterizing their property through various spectroscopic and microscopic techniques followed by measuring their performance to be suitable for real application after coin cell fabrication.
In the first part of this study, hybrid nanostructured microporous carbon-mesoporous carbon doped titanium dioxide/sulfur composite (MC-Meso C-doped TiO2/S) was we designed as a cathode material for Li-S batteries. The hybrid MC-Meso C-doped TiO2 host material was produced by a low-cost hydrothermal and annealing process. It found that the resulting conductive material showed dual microporous and mesoporous behavior, which enhanced the effective trapping of sulfur and polysulfides. The hybrid MC-Meso C-doped TiO2/S composite material possessed rutile TiO2 nanotube structure with successful carbon doping, while sulfur was uniformly distributed in the hybrid MC-Meso C-doped TiO2 composite materials after the melt-infusion process. Electrochemical measurements of the hybrid cathode material also showed improved cycling stability and rate performance with high sulfur loading (61.04 wt %). Moreover, the material delivered an initial discharge capacity of 802 mAh g-1 and maintained at 578 mAh g-1 with the coulombic efficiency greater than 97.1% after 140 cycles at 0.1 C
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rates. This improvement was thought to be attributed to the unique hybrid nanostructure of the MC-Meso C-doped TiO2 host and the good dispersion of sulfur in the narrow pores of the spherical microporous carbon (MC) and the Meso C-doped TiO2 nanotube support.
Secondly, the novel nanocomposite cathode materials consisting of sulfur (80 wt%) embedded within nitrogen doped three-dimensional reduced graphene oxide (N-3D-rGO) was designed by a controllable sulfur impregnation method. Nitrogen doping helped to increase the surface area by ten times and pore volume by seven times from pristine graphene. These structural features allowed the cathode to accommodate more sulfur. Moreover, the cathode adsorbed polysulfides and prevented their detachment from host materials, thereby achieving stable cycle performance. The solution drop sulfur impregnation method provided uniform distribution of nanosized sulfur in a controlled manner. Furthermore, the cathode delivered high initial discharge capacities of 1042 mAhg-1 and 916 mAh g-1 at 0.2 C and 0.5 C with excellent capacity retention of 94.8% and 81.9% after 100 cycles respectively, with a low decay rate of 0.062% per cycle after 500 cycles. Thus, the combination of solution drop sulfur impregnation and nitrogen doping opens a new chapter for resolving capacity fading, as well as long cycling problems, and creates a new strategy to increase sulfur loading in controlled mechanism.
In the final part of this dissertation, a novel design of dual-confined sulfur cathode with core-shell architecture, where sulfur (72.5 wt%) was first encapsulated in MC cores and embedded by graphene (G) shells was reported. Larger, soluble polysulfide intermediates (Li2Sx, 4≤x≤8) were trapped by G shells, which prevented the dissolution of soluble polysulfide intermediates into the organic electrolyte, so that a stable cycling
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performance could be achieved. Moreover, the G shell created the hollow space in-between, which helped ensure the integrity of the hybrid cathode against the volume expansion upon cycling. On the other hand, MC confined smaller sulfur (S2-4) molecules within its small pores and suppressed the formation of soluble polysulfides. The resulting electrode delivered a high initial discharge capacity of 982 mAh g-1 with enhanced capacity retention of 85.4% after 100 cycles at 0.2 C rates. More importantly, the cathode exhibited a high discharge capacity of 886 mAh g-1, and maintained at 601 mAh g-1 after 500 cycles at 0.5 C with the coulombic efficiency of nearly 100%, which is the best performance among reported cycle stabilities.

摘要 ............................................................................................................................ i
Abstract ....................................................................................................................iii
Acknowledgments ................................................................................................... vi
Table of contents .................................................................................................. viii
List of Figures ...................................................................................................... xiii
List of Tables ......................................................................................................... xxi
List of schemes ..................................................................................................... xxii
List of units and Abbreviations ........................................................................ xxiii
Chapter 1: Background .......................................................................................... 1
1. Energy and Energy Sources .......................................................................... 1
2. Types of Battery ............................................................................................ 2
Chapter: Introduction ............................................................................................. 4
1. Lithium-Sulfur Battery .................................................................................. 4
2. Principles and Limitations of Lithium-Sulfur Batteries ............................... 6
2.1. Principles ................................................................................................................ 6
2.2. Limitation of lithium-sulfur batteries ..................................................................... 8
2.2.1. Poor electronic conductivity .............................................................................. 8
2.2.2. Dissolution of polysulfides and shuttle effect .................................................... 8
2.2.3. Large volume expansion .................................................................................... 9
2.2.4. Dendrite formation ........................................................................................... 10
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3. Components of Lithium-Sulfur Battery ...................................................... 11
3.1. Anode materials .................................................................................................... 11
3.2. Electrolytes ........................................................................................................... 12
3.3. Separators ............................................................................................................. 12
3.4. Cathode materials ................................................................................................. 13
3.4.1. Carbon-sulfur cathode ...................................................................................... 13
3.4.2. Metal oxide supported sulfur cathode composite ............................................ 17
3.4.3. Graphene-sulfur composite .............................................................................. 18
4. Motivation and Objectives of the study ...................................................... 22
4.1. Motivations ........................................................................................................... 22
4.2. Objectives ............................................................................................................. 23
Chapter 3: Experimental Section and Characterization ................................... 25
1. General Experimental Section .................................................................... 25
1.1. Chemicals and regents .......................................................................................... 25
1.2. Synthesis of Meso C-doped TiO2 nanotubes ........................................................ 26
1.3. Preparation of MC and hybrid nanostructured MC-Meso C-doped TiO2 ............ 27
1.4. Synthesis of hybrid nanostructured MC-Meso C-doped TiO2/S composite cathode .................................................................................................................. 27
1.5. Synthesis of graphene oxide (GO) ....................................................................... 28
1.6. Synthesis of 3D-rGO and N-3D-rGO host materials ........................................... 28
1.7. Synthesis of S@N-3D-rGO nanocomposites ....................................................... 29
1.8. Synthesis of S/MC composites ............................................................................. 30
1.9. Synthesis of core-shell G@S/MC nanocomposites .............................................. 30
2. Structure Characterization ........................................................................... 31
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2.1. Physical characterization techniques (XRD, Raman,SEM, TEM, FT-IR, XPS, EDS, BET, TGA ................................................................................................... 31
3. Computational Details ................................................................................. 33
Chapter 4: Design of Hybrid Nanostructured Microporous Carbon-Mesoporous Carbon Doped TiO2/Sulfur Composite Cathode Materials for Rechargeable Lithium-Sulfur Batteries ............................................................................................. 35
1. Introduction ................................................................................................. 35
2. Results and Discussion................................................................................ 38
2.1. Material characterization ...................................................................................... 38
2.2. The electrochemical performance ........................................................................ 55
2.2.1. Cyclic voltammetry test ................................................................................... 55
2.2.2. Galvanostatic charge-discharge test ................................................................. 58
2.2.3. Cycle stability test ............................................................................................ 61
2.2.4. Rate capability test ........................................................................................... 65
2.2.5. Electrochemical impedance spectroscopy (EIS) test ....................................... 68
3. Summary ..................................................................................................... 71
Chapter 5: Controllable Embedding of Sulfur in High Surface Area Nitrogen Doped Three Dimensional Reduced Graphene Oxide host by Solution Drop Impregnation Method for High Performance Lithium-Sulfur Batteries ................................. 72
1. Introduction ................................................................................................. 72
xi
2. Results and Discussion................................................................................ 74
2.1. Material characterization ...................................................................................... 74
2.2. Electrochemical performance ............................................................................... 90
2.2.1. Cyclic voltammetry and galvanostatic charge-discharge test .......................... 90
2.2.2. Cycle stability and rate capability test ............................................................. 93
2.2.3. Electrochemical impedance spectroscopy (EIS) test ....................................... 98
2.2.4. Computational result ........................................................................................ 99
2.2.5. Post-mortem studies ....................................................................................... 102
3. Summary ................................................................................................... 105
Chapter 6: Dual-Confined Sulfur in Hybrid Nanostructured Materials for Enhancement of Lithium-Sulfur Battery Cathode Capacity Retention .......................................................... 106
1. Introduction ............................................................................................... 106
2. Results and Discussion.............................................................................. 108
2.1. Material characterization .................................................................................... 108
2.2. Electrochemical performance ............................................................................. 123
2.2.1. Cyclic voltammetry and galvanostatic charge-discharge test ........................ 123
2.2.2. Cycle stability and rate capability test ........................................................... 126
2.2.3. Electrochemical impedance spectroscopy (EIS) test ..................................... 131
3. Summary ................................................................................................... 134
Chapter 7: Conclusions and Future outlooks ................................................... 135
1. Conclusions ............................................................................................... 135
xii
2. Future Outlooks ......................................................................................... 138
Appendices ............................................................................................................ 139
A. Supporting datas for Approach-I .............................................................. 139
B. Supporting datas for Approach-II ............................................................. 141
C. Supporting datas for Approach-III ............................................................ 145
References ............................................................................................................. 146
List of Research Papers ....................................................................................... 173
Conference/Workshop Presentations ................................................................ 174
                                

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