本篇論文旨在探討如何在鋰離子電池的電解質中建立鋰離子傳導通道，以改善固態電解質的低離子電導度和低鋰離子傳導數的問題。為了實現這一目標，將單離子導體電解質Lithium 4-styrenesulfonyl(phenylsulfonyl)imide (SPSILi)經由原子轉移自由基聚合法(ATRP)將其接枝於碳奈米管表面，在碳奈米管表面建立具有鋰離子傳導能力的連續區域，再將之作為添加劑，添加到凝膠態高分子電解質和全固態高分子電解質中。由於碳奈米管表面具有磺醯亞胺官能基團，與鋰離子之間存在相互吸引力，因此在表面可以形成傳輸鋰離子的通道，從而提升離子電導度和鋰離子傳導數。
所合成的單離子導體電解質SPSILi以傅立葉轉換紅外光譜儀(FTIR)和核磁共振光譜(1H NMR)鑑定其結構，其高分子鏈改質的碳奈米管(CNT-SPSILi)以FTIR、拉曼光譜儀(Raman)、X-光光電子能譜圖(XPS)、高解析度穿透式電子顯微鏡(HRTEM)等鑑定其結構和性質經由熱重分析儀(TGA)的分析，CNT-SPSILi的SPSILi高分子鏈含量為32 wt%。將CNT-SPSILi作為添加劑以特定濃度添加到高分子電解質基材中，據以製備具有良好分散性的凝膠態高分子電解質和全固態高分子電解質，其中凝膠態電解質使用PEGDMA作為基材，全固態電解質使用PEO作為基材。
對以PEGDMA作為基材的凝膠態電解質進行電化學測試，結果顯示其具有1.5*10-3 S/cm的離子電導度，相較於未添加任何添加劑的凝膠態電解質，離子電導度提升了5倍，鋰離子傳導數也由0.51提升至0.68。在電池性能方面，在0.2C的充放電速率下，添加改質碳奈米管後的電池容量從107.8 mAh g-1增加到138.2 mAh g-1，在2 C的高速充放電速率下，仍能維持98.7 mAh g-1的電池容量。此外，在對稱鋰金屬的電池測試中，添加改質碳奈米管可以提供更好的長期穩定性。這些結果表明，將單離子導體電解質高分子接枝到碳奈米管上可以有效形成鋰離子傳導通道，有助於鋰離子的傳導。
另外，對以PEO作為基材的全固態電解質進行電化學測試，結果顯示其具有5.14*10-4 S/cm的離子電導度，相較於未添加任何添加劑的全固態電解質，離子電導度提升了4倍，鋰離子傳導數也由0.27提升至0.32。在電池性能方面，在2 C的高速充放電速率下，仍能維持138.2 mAh g-1的電池容量。在長期的充放電循環測試中，在1 C的充放電速率下，相較於未添加填料的固態電解質，添加改質碳奈米管的固態電解質將電池容量提升至137.2 mAh g-1，並在經過600圈後仍保持在129.5 mAh g-1，維持了最高電容量的94.4 %。此外，在對稱鋰金屬的電池測試中，添加改質碳奈米管可以降低界面阻抗，形成更穩定的電極介面層。這些結果與使用PEGDMA基材的凝膠態電解質相似，證明單離子導體電解質高分子接枝於碳奈米管上可以有效形成鋰離子傳導通道，有效的幫助鋰離子傳導，使其更符合快速充放電的電池所需。

This research aims to investigate the establishment of lithium ion conducting pathways within the electrolyte of lithium ion batteries, with the goal of addressing the issues of low ionic conductivity and low lithium ion conduction number in solid-state electrolytes. To achieve this objective, the single-ion conductor electrolyte, Lithium 4-styrenesulfonyl(phenylsulfonyl)imide (SPSILi), is grafted onto the surface of carbon nanotubes using atom transfer radical polymerization (ATRP). Creating continuous regions on the carbon nanotube surface with lithium ion conduction capabilities. These modified nanotubes are subsequently employed as additives in gel polymer electrolytes and all-solid-state polymer electrolytes. This enhances ion conductivity and lithium transference number.
The synthesized single-ion conductor electrolyte, SPSILi, is structurally characterized using Fourier-transform infrared spectroscopy (FTIR) and proton nuclear magnetic resonance spectroscopy (1H NMR). The modified carbon nanotubes (CNT-SPSILi) are characterized for their structure and properties using techniques such as FTIR, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and high-resolution transmission electron microscopy (HRTEM). Thermal gravimetric analysis (TGA) indicates that CNT-SPSILi contains 32 wt% of SPSILi polymer chains.
Incorporating CNT-SPSILi as an additive in specific concentrations to polymer electrolyte matrices results in well-dispersed gel and all-solid-state polymer electrolytes. Polyethylene glycol dimethacrylate (PEGDMA) serves as the matrix for gel polymer electrolytes(GPE), while polyethylene oxide (PEO) is used for all-solid-state polymer electrolytes(SPE).
Electrochemical testing of the GPE based on PEGDMA reveals an ion conductivity of 1.5*10-3 S/cm. The ion conductivity is five times higher compared to the GPE without any additives. Additionally, lithium transference number improves from 0.51 to 0.68. Battery performance tests at 0.2C discharge/charge rate demonstrate that the capacity of batteries with modified carbon nanotubes increases from 107.8 mAh g-1 to 138.2 mAh g-1. Even at a higher 2C discharge/charge rate, the battery capacity still remains at 98.7 mAh g-1. Notably, in symmetric lithium metal battery tests, the inclusion of modified carbon nanotubes enhances long-term stability.
Similarly, for SPE using PEO as the matrix, electrochemical tests reveal an ion conductivity of 5.14*10-4 S/cm. The ion conductivity is four times higher compared to the SPE without any additives. Lithium transference number also increases from 0.27 to 0.32. At a higher 2C discharge/charge rate, the battery capacity remains at 138.2 mAh g-1. Long-term cycling tests at 1C discharge/charge rate demonstrate that the SPE with modified carbon nanotubes achieves a battery capacity of 137.2 mAh g-1, maintaining 129.5 mAh g-1 after 600 cycles, representing 94.4% of the highest capacity. Moreover, in symmetric lithium metal battery tests, the inclusion of modified carbon nanotubes reduces interface impedance, leading to a more stable electrode interface layer.
These outcomes indicate that grafting the single-ion conductor polymer electrolyte on carbon nanotubes effectively creates lithium ion conduction pathways, facilitating lithium ion transport to meet the requirements of fast charge and discharge in batteries.
 

摘要 i
Abstract iii
目錄 v
圖目錄 x
表目錄 xiv
第1章 緒論 1
1.1 前言 1
1.2 二次電池的發展歷史 2
1.2.1 鉛酸電池 3
1.2.2 鎳鎘電池 4
1.2.3 鎳氫電池 5
1.3 鋰離子電池 6
1.3.1 電極材料 8
1.3.2 隔離膜 11
1.4 鋰離子電池中的電解質 12
1.4.1 液態電解質 12
1.4.2 固態電解質 13
1.4.3 無機陶瓷電解質 14
1.4.4 高分子電解質 17
1.5 研究動機 19
第2章 文獻回顧 20
2.1 鋰離子傳導數的改善方法 21
無機陶瓷材料 21
單離子導體 22
2.2 提升離子電導度的方法 25
高分子結構設計 25
無機陶瓷材料 27
建立離子通道 27
2.3 研究方法 36
第3章 實驗方法 39
3.1 實驗藥品與溶劑 39
3.2 實驗儀器 41
3.3 實驗步驟 44
3.3.1 單離子傳導單體Lithium 4-styrenesulfonyl(phenylsulfonyl)imide (SPSILi)之合成 44
3.3.2 利用ATRP之方法將SPSILi改質CNT表面 45
3.3.3 添加不同填料之PEGDMA凝膠態電解質製備 46
3.3.4 添加不同填料之PEO固態電解質製備 47
3.3.5 離子電導度測量 47
3.3.6 電化學穩定性測量 48
3.3.7 對稱鋰金屬電極充放電循環 49
3.3.8 電池效能測試 50
第4章 結果與討論 51
4.1 單離子傳導單體Lithium 4-styrenesulfonyl(phenylsulfonyl)imide (SPSILi)之鑑定 51
4.2 利用SPSILi改質CNT表面之合成 53
4.3 SPSILi改質CNT之鑑定 54
Raman Spectrum 54
FTIR Spectrum 55
XPS 56
HRTEM 59
TGA 60
分散性 61
4.4 複合PEGDMA凝膠態高分子電解質之膜材 63
4.5 複合PEGDMA凝膠態高分子電解質之電化學性質測試 66
離子電導度測量 66
電子電導度測量 68
鋰離子傳導數測量 69
電化學穩定性測試 70
4.6 複合PEGDMA凝膠態高分子電解質之電池性能測試 71
電池充放電速率測試 71
對稱鋰金屬電池表現 72
4.7 複合PEO全固態高分子電解質之膜材 74
4.8 複合PEO全固態高分子電解質之電化學性質測試 76
離子電導度測量 76
電子電導度測量 83
鋰離子傳導數測量 84
電化學穩定性測試 85
4.9 複合PEO全固態高分子電解質之電池性能測試 87
電池充放電速率測試 87
長期循環充放電測試 89
對稱鋰金屬電池測試 93
第5章 結論與展望 95
第6章 參考文獻 96

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