臺灣博碩士論文加值系統

本研究採用商用人造石墨（MAGE-3）作為負極材料的基材，並以噴霧乾燥法及化學沉澱法進行表面改質，將MAGE-3表面分別摻入Nb2O5、ZnO及NiO元素，合成出MA-Nb、MA-Zn及MA-Ni複合負極材料，藉以改善其電化學性能。結晶繞射圖譜（XRD）結果顯示改質後的材料仍保持石墨碳本身的結構，且同時存在改質氧化物的特徵峰。顆粒尺寸分布（SLS）、表面形態分析（SEM）及能量散射光譜（EDS）分析結果顯示，改質元素均勻分布於石墨碳顆粒表面，且表面改質對於石墨顆粒尺寸並無顯著影響。
電化學性能結果顯示，MAGE-3-Bare、MA-Nb、MA-Zn及MA-Ni經過100次充/放循環後，Li+脫出容量分別為284 mAh/g、364 mAh/g、330 mAh/g及357 mAh/g，電容量維持率分別為81.18 %、100 %、92.71 %及99.25 %。研究發現，石墨碳材經金屬氧化物改質後，形成的氧化物顆粒與石墨碳界面緊密連接，具有緩衝及支撐結構的作用，並可減緩Li+嵌入/脫出過程中所導致的體積膨脹。其中，在氮氣氣氛下並以630 ℃燒結處理後所形成的複合材料，由於Nb2O5與石墨碳之間產生的相互作用，經過充/放電循環後，可以有效緩解體積收縮/膨脹，維持複合材料的結構穩定性。此外，Nb2O5顆粒可提升電導率，提供更快速的電子轉移路徑，因而優化石墨碳材的電化學性能。
除了半電池測試外，研究中還以TiO2-LNMO作為正極，改質與未改質石墨碳材料作為負極，組裝成CR-2032型全電池進行充/放電測試。將經過100次充/放循環後拆解電池，並對正/負極電極進行拉曼光譜（Raman）及X射線能譜（XPS）分析。結果得知，透過Nb2O5表面改質後，石墨碳表面形成了保護層，使其結構保持高度有序，並有效抑制材料表面與電解液的過度反應，減少因正極錳離子溶出所造成的副反應，保持材料結構的穩定性，因而顯著使電化學性能提升。

Commercial artificial graphite (MAGE-3) was used in this study as the substrate material for the negative electrode. Surface modification was carried out using the spray drying method and the chemical precipitation method to add Nb2O5, ZnO, and NiO to the MAGE-3 surface in order to synthesize the MA-Nb, MA-Zn, and MA-Ni composite negative electrode materials, respectively, to improve electrochemical performance. The result for the X-ray diffraction (XRD) crystallization pattern indicated that the modified material was able to maintain the structure of graphitic carbon and had characteristic peaks of the modified oxides. Further, the results for the particle size distribution (SLS), surface morphology analysis (SEM), and energy scattering spectroscopy (EDS) demonstrated that the modified elements were uniformly distributed across the surface of the graphite’s carbon particles and that the surface modification had no significant effect on the graphite’s particle size.
The electrochemical performance revealed that the MAGE-3-Bare, MA-Nb, MA-Zn, and MA-Ni had a capacitance of 284, 364, 330, and 357 mAh/g, respectively, after 100 cycles of charging and discharging. Furthermore, the capacity maintenance rates were 81.18%, 100%, 92.71%, and 99.25%, respectively. It was found that the formed oxide particles were closely connected to the graphitic carbon interface after the graphite carbon material had been modified by the metal oxides, producing a cushioning and supporting structure to slow down the volume expansion caused by the Li+ embedding and removal processes. The composite material, which was manufactured through sintering at 630℃ in a nitrogen atmosphere, was able to effectively alleviate the volume shrinkage and expansion after charging and discharging cycles owing to the interaction between Nb2O5 and graphite carbon. This enabled the maintenance of the structural stability of the composite material. Moreover, the Nb2O5 particles enhanced electrical conductivity and provided a faster transfer path for electrons, thus optimizing the electrochemical performance of the graphite carbon material.
In addition to the half-cell test, TiO2-LNMO was used as the cathode, while the modified and unmodified graphitic carbon materials were used as the anode to assemble a CR-2032 full cell for a charging and discharging test. The battery was disassembled after 100 charging and discharging cycles, and Raman spectroscopy and X-ray spectroscopy (XPS) analyses were conducted for the anode and cathode. The results demonstrated that the surface modification with Nb2O5 led to the production of a protective layer on the graphite carbon surface that keeps the structure highly organized and effectively inhibits over-interaction between the material surface and the electrolyte. This effect can reduce the secondary reaction caused by the dissolution of the positive manganese ions at the cathode and can help maintain the stability of the material structure, thereby significantly improving electrochemical performance.

摘要...i
Abstract...ii
誌謝...iv
目錄...v
表目錄...ix
圖目錄...x
第一章 緒論...1
1.1 前言...1
1.2 研究動機...1
第二章 文獻回顧...2
2.1 鋰離子電池簡介...2
2.1.1 鋰離子電池工作原理...3
2.1.2 鋰離子電池的特性...4
2.1.4 鋰離子電池的關鍵材料組成...5
2.2 正極材料...5
2.2.1 LiCoO2（LCO）...6
2.2.2 LiNiO2（LNO）...7
2.2.3 LiMn2O4（LMO）...8
2.2.4 LiNi0.5Mn1.5O4（LNMO）...9
2.2.5 小結...9
2.3 有機電解液...10
2.4 隔離膜...10
2.5 負極材料...11
2.5.1 碳基材料...11
2.5.2 鈮基材料...14
2.5.3 過渡金屬氧化物...15
2.5.4 小結...16
2.6 金屬氧化物合成方法...17
2.6.1 水熱合成法（hydrothermal method）...17
2.6.2 沉澱法（precipitation method）...17
2.6.3 噴霧乾燥法（spray drying）...17
2.6.4 溶膠-凝膠法（sol-gel method）...18
2.6.5 固相合成法（solid-state reaction）...18
2.7 以金屬氧化物修飾碳基材料...19
2.7.1 鈮酸鈦（TiNb2O7）...19
2.7.2 氧化鋅（ZnO）...21
2.7.3 一氧化鎳（NiO）...23
2.7.4 一氧化錳（MnO）...25
2.7.5 二氧化鈦（TiO2）...27
2.7.6 氧化矽（SiOx）...30
第三章 實驗材料與方法...34
3.1 實驗材料與儀器...34
3.1.1 實驗材料...34
3.1.2 實驗儀器...35
3.2 實驗架構流程圖...36
3.2.1 金屬氧化物表面改質MAGE-3石墨粉體...36
3.2.2 挑選改質性能最佳的氧化物優化製程熱處理氣氛與溫度...37
3.2.3 搭配高電壓尖晶石型LiNi0.5Mn1.5O4正極材料組裝成全電池...38
3.3 實驗方法與步驟...39
3.3.1 酸液處理MAGE-3石墨粉體...39
3.3.2 Nb2O5表面改質MAGE-3石墨粉體...39
3.3.3 ZnO表面改質MAGE-3石墨粉體...40
3.3.4 NiO表面改質MAGE-3石墨粉體...40
3.3.5 材料燒結...41
3.3.6 負極材料漿料調配及極板製備...41
3.3.7 鈕扣型電池組裝...43
3.4 材料物理性質分析...44
3.4.1 X光繞射儀 （X-ray Diffraction）...44
3.4.2 場發射電子顯微鏡（Field Emission Scanning Electron Microscope）...44
3.4.3 能量色散X射線譜（Energy-dispersive X-ray spectroscopy）...44
3.4.4 雷射粒徑分析儀（Static Light Scattering Method）...45
3.4.5 X射線光電子能譜儀（X-ray photoelectron spectroscopy）...45
3.4.6 拉曼光譜儀（Raman spectroscopy）...45
3.5 電化學性能分析...46
3.5.1 充放電測試...46
3.5.2 交流阻抗頻譜分析（AC impedance）...47
3.5.3 循環伏安法（cyclic voltammetry）...47
第四章 實驗結果與討論...48
4.1 不同金屬氧化物改質石墨碳基材料...49
4.1.1 晶體結構分析...49
4.1.2 顆粒尺寸及表面形態分析...50
4.1.3 拉曼光譜分析...55
4.1.4 循環伏安法...57
4.1.5 倍率性能測試...60
4.1.6 循環性能測試...63
4.1.7 高溫循環性能測試...65
4.1.8 交流阻抗測試...67
4.1.9 小結...69
4.2 不同燒結條件之Nb2O5改質石墨碳...70
4.2.1 晶體結構分析...70
4.2.2 顆粒尺寸及表面形態分析...71
4.2.3 拉曼光譜分析...77
4.2.4 倍率性能測試...79
4.2.5 循環性能測試...83
4.2.6 交流阻抗測試...85
4.2.7 小結...87
4.3 最佳改質負極材料組裝成CR-2032型全電池...88
4.3.1 倍率性能測試...89
4.3.2 循環性能測試...92
4.3.3 交流阻抗測試...94
4.3.4 電極截面SEM分析...96
4.3.5 拉曼光譜分析...97
4.3.6 X射線光電子能譜分析...100
第五章 結論...101
第六章 未來展望...103
參考文獻...104
Extended Abstract...110

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