為了改善鋰離子電池(Lithium Ion Batteries, LIBs)的缺點，近年來對於裝置的改進研究受到了許多關注，其中鋰離子電容器(Lithium Ion Capacitors, LICs)與鋰硫電池(lithium-sulfur batteries)便吸引了眾多研究的目光。鋰離子電容器屬於同時擁有電池陽極以及電容陰極的混合式電容器(hybrid capacitor)，可同時結合鋰離子電池與超級電容器的優點，在擁有高能量密度的同時還可提供媲美超級電容器的功率密度與循環穩定性；鋰硫電池則使用硫取代一般鈷酸鋰類的陰極材料，硫具有相較於鈷酸鋰等陰極材料高出許多的理論電容(~ 1675 mAh g-1)與能量密度(~ 2600 Wh kg-1)，亦被視為下一代鋰離子電池性能升級的關鍵所在。針對兩種儲能裝置各自需要被改善的問題，本研究對於鋰離子電容器陽極與鋰硫電池陰極進行改進與發展。
在鋰離子電容器方面，本研究著重對於其中擁有電池性能的陽極進行探討。商業化石墨陽極理論電容值(≈ 372 mAh g-1)較低，無法提供更高的能量密度，因此近年亦有許多開發新陽極材料之研究。在眾多材料當中，矽碳複合材料成為下一世代鋰離子電池發展的首要目標，在鋰離子電池陽極中矽擁有相當高的理論電容值(≈ 4200 mAh g-1)，並且其含量豐富、脫鋰電位低等優點也使其成為優秀的陽極材料。但矽的導電性不佳，而且在充放電過程中大量的體積變化也成為當今研究者們努力要克服的難題，所以大部分研究在陽極中會使用矽碳複合材料而非純矽材料，以增加陽極的導電性並降低整體的體積膨脹率。本研究以具介孔之矽奈米微粒複合摻氮碳材作為陽極，藉由介孔提供矽材料體積膨脹的空間，摻氮碳材提高陽極之導電性及穩定性，並且使用具有高比表面積之活性碳作為陰極。組合出之鋰離子電容器在0.32 kW kg-1的功率密度下可以提供高達210 Wh kg-1的能量密度，且在36.1 kW kg-1的高功率密度下仍能保有70.1 Wh kg-1的能量密度，在文獻中表現突出，並在經過20,000次循環的長效性測試後，還能保有原本89%的能量密度，具有相當優異之循環穩定性。
鋰硫電池雖然具有相當高的理論電容量與能量密度，但是仍然面臨許多限制。首先硫本身的導電性不佳，且在反應過程中所產生的多硫化鋰更因為其可溶於電解液的特性而可能擴散到陽極與鋰金屬接觸，產生活性物質的損耗甚至是短路的危害。對於這些缺點多數的研究選擇加入基底材料(sulfur host)來解決問題。初期基底材料的選擇通常為多孔碳材，因其具有良好的導電性，並且具有孔洞可以阻礙多硫化物擴散到陽極，但不具極性的純碳材與具極性的多硫化鋰彼此之間交互作用並不強烈，因此在經過多次循環之後容量仍然會產生明顯的衰退。有鑑於此更多具有極性的材料被報導使用於鋰硫電池中，其中金屬硫化物因為與多硫化物具有強烈的化學吸附力、與其它極性材料相比具有較好的導電性且具有催化多硫化物氧化還原反應之效果而被廣泛地研究。本研究利用類普魯士藍化合物衍生之三元金屬硫化物複合摻氮碳奈米盒，結合鐵、鈷、鎳硫化物各自的優點並且利用氨水加以蝕刻造孔以增加比表面積，成功達成快速吸附多硫化物以及減少鋰離子質傳阻礙的效果。將其作為鋰硫電池陰極，其儲能表現在0.1 C充放電速率下可以提供1238 mAh g-1的容量，在2 C時仍保有655 mAh g-1的容量，此外以1 C的充放電速率進行200個循環的穩定性測試後，仍然保有575 mAh g-1的容量，平均每次循環的容量損失率僅為0.049%。

Lithium ion batteries (LIBs) are currently the most popular energy storage device, but there are still ample rooms for improvements and new lithium ion based energy storage devices are under intensive development. Among them, lithium ion capacitors (LICs) and lithium-sulfur batteries (LSBs) have attracted much research attention. Lithium-ion capacitors are a hybrid energy storage device, composed of a battery type anode and a capacitor type cathode to take advantages of both lithium-ion batteries and supercapacitors (SCs) in one. While possessing high energy densities as in LIBs, LICs also provide high power densities and long-term stability comparable to SCs. LSBs use sulfur instead of the common lithium cobalt oxides of LIBs as the cathode material. Sulfur has a much higher theoretical capacity (~ 1675 mAh g-1) and energy density (~ 2600 Wh kg-1) than the popular cathode materials of LIBs such as lithium cobalt oxides, and is regarded as the key to the next generation lithium ion based energy storage. This work focuses on development of anode materials for LICs and cathode materials for LSBs.
As an anode material, silicon has a very high theoretical capacitance (≈ 4200 mAh g-1) and its delithiation potential is low, making it an outstanding anode material, but its poor conductivity and large volume variations involved during charging/discharging cycles are two detrimental issues to be resolved for its commercial applications. Most researchers use silicon/carbon composites rather than pure silicon as the anode to increase the conductivity and to reduce the overall volume variation. In this study, mesoporous silicon nanoparticles composited with N-doped carbon materials (m-Si@NDC) are developed as the anode for Li-ion based energy storage. Here, the buffer space to accommodate the volume variation of Si during charging/discharging cycles is provided by the mesopores of the mesoporous silicon nanoparticles, and N-doped carbon materials improve the conductivity and stability of the anode. Besides, activated carbons with high surface areas are used as the cathode for LIC assembly. The thus assembled LIC delivers a high energy density of 210 Wh kg-1 at a power density of 0.32 kW kg-1, and maintains a decent energy density of 70.1 Wh kg-1 even at a high power density of 36.1 kW kg-1. The performance is outstanding as compared with those reported in the literature. After the long-term test of 20,000 cycles, it retains 89% of the original energy density, indicating its excellent cycling stability.
LSBs, although possessing a relatively high theoretical electrical capacity and energy density, still face many limitations. First of all, the conductivity of sulfur is poor, and the lithium polysulfides generated during the discharge process may dissolve in the electrolyte and diffuse to the anode, resulting in loss of active materials and even short circuiting. For these shortcomings, most researchers choose to add sulfur hosts to solve the problem. In this work, Prussian blue analogues (PBAs) derived trimetallic sulfides composited with N-doped carbon nanoboxes are successfully synthesized, in which ammonia is used to etch the eight corners of the cubic structure of PBAs to create extra pores and increase the reaction surface area to boost adsorption of polysulfides and to improve the mass transfer of electrolyte in and out the nanoboxes. The as fabricated cathode delivers a discharge capacity of 1238 mAh g-1 at 0.1 C, and maintains a capacity of 655 mAh g-1 at 2 C. In addition, after a 200-cycle stability test at 1 C, it still retains a capacity of 575 mAh g-1, giving a low capacity decay rate of only 0.049% per cycle.

摘要 I
誌謝 V
目錄 VI
圖目錄 IX
表目錄 XV
第1章 簡介 1
1-1 緒論 1
1-2 鋰離子電池 2
1-3 鋰離子電容器 5
1-4 鋰硫電池 6
1-5 多巴胺聚合簡介 8
1-6 鎂熱還原簡介 9
1-7 研究動機 10
1-7-1 以具介孔碳矽複合奈米微粒應用於鋰離子電容器 10
1-7-2 以類普魯士藍衍生三元金屬硫化物應用於鋰硫電池 11
第2章 文獻回顧 13
2-1 鋰離子電容器 13
2-1-1 概述 13
2-1-2 多孔矽奈米柱設計 15
2-1-3 利用網狀電極與摻氮碳材組成對稱式鋰離子電容器 18
2-1-4 以含孔洞結構矽材使用於鋰離子電容器 22
2-2 鋰硫電池 26
2-2-1 概述 26
2-2-2 中空硫化鎳複合碳材 26
2-2-3 二元金屬硫化物複合奈米碳管 28
第3章 實驗方法與儀器 31
3-1 實驗藥品 31
3-2 實驗儀器 34
3-3 分析儀器 35
3-4 實驗步驟 37
3-4-1 以具介孔矽奈米微粒複合氮摻雜碳材應用於鋰離子電容器 37
3-4-2 以三元金屬硫化物複合經蝕刻奈米碳盒應用於鋰硫電池 40
3-5 電化學測試與分析 42
第4章 結果與討論-鋰離子電容器部分 45
4-1 具介孔之二氧化矽球 45
4-2 摻氮碳材包覆二氧化矽奈米球 47
4-3 以鎂熱還原法還原MSS@NDC 48
4-3-1 鎂熱反應條件的控制 48
4-3-2 m-Si@NDC材料鑑定 51
4-4 m-Si@NDC陽極半電池電化學測試 58
4-4-1 不同反應時間m-Si@NDC比較 58
4-4-2 有無介孔對於長效穩定性之影響 59
4-4-3 針對m-Si@NDC其它電化學分析 60
4-4-4 原位拉曼測試 62
4-5 萄萄糖衍生之活化碳球(GCNS)材料鑑定 63
4-6 GCNS陰極半電池電化學測試 65
4-7 m-Si@NDC//GCNS鋰離子電容器測試 67
4-7-1 最佳重量配比測試 67
4-7-2 電容表現測試 67
4-7-3 循環長效性測試 69
4-7-4 與近年文獻中鋰離子電容器之比較 70
第5章 結果與討論-鋰硫電池部分 73
5-1 三元金屬(鐵、鈷、鎳)類普魯士藍 73
5-2 三元金屬硫化物複合氮摻雜碳奈米盒(S-FeCoNi@C-CNB)材料鑑定與分析 76
5-2-1 形貌、晶格繞射與元素組成分析 76
5-2-2 有無造孔比較 79
5-2-3 XPS分析 80
5-2-4三元金屬硫化物與純硫之複合材料(S-FeCoNi@C-CNB/S) 82
5-2-5 多硫化鋰吸附測試 84
5-3 S-FeCoNi@C-CNB/S應用於鋰硫電池陰極電化學測試 85
5-3-1 電池容量表現 85
5-3-2 循環長效表現測試 87
5-3-3 鋰離子質傳係數比較 89
5-3-4 與其它文獻鋰硫電池比較 92
第6章 結論 94
參考文獻 95

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