臺灣博碩士論文加值系統

利用噴霧乾燥法製備氯摻雜及鋰過量之 LiNi0.5Mn1.5O4 （LNMO） 基正極材料，探討氯摻雜及鋰過量對 LNMO 基正極材料的表面形貌、結晶結構及電化學特性的影響。由 SEM 圖譜及 PSA 數據可得知，氯摻雜及鋰過量對合成之粉末的表面形貌及粒徑大小並無顯著的影響。而透過 X 光繞射圖譜可發現，適量的氯摻雜於 LNMO 中會增加材料的晶格常數，並可有效抑制岩鹽雜相的生成；另一方面，過量的鋰摻雜於 LNMO 之中亦會擴大材料的晶格，然而，鋰過量會增加岩鹽雜相的生成，阻礙鋰離子的擴散。由傅立葉轉換紅外光譜可得知，氯摻雜及鋰過量的 LNMO 在900oC 的燒結溫度下皆會形成主要結構為 Fd3 ̅m 的無序相；然而透過計算 586/624 波段能帶的比值經比較後可發現，LNMO 會隨著氯摻雜的增加提升有序程度；相反地，鋰過量則會降低過渡金屬於晶體中的有序程度，使材料偏向無序之 Fd3 ̅m 相。
由循環充放電測試結果及靜置溶出實驗發現，適量的氯摻雜於 LNMO 中可提升電容量及倍率性能，並可抑制過渡金屬離子溶出，降低電解液被加速氧化分解的機會，使其在高溫循環下能有較佳的庫倫效率及循環壽命。然而，過量的鋰摻雜於 LNMO 中則會降低電化學性能表現，其較差的電化學性能表現與生成較多雜相阻礙鋰離子擴散有關。

The chlorine-doping and lithium-excess of LiNi0.5Mn1.5O4 (LNMO) - based cathode materials were prepared by spray-drying method, and their effects on the surface morphology, crystal structure, and electrochemical properties were investigated. From the SEM and PSA data, it was found that the surface morphology and particle size of the synthesized powders were not affected by the doping of chlorine and the excess of lithium ions. It was observed by XRD patterns that the chlorine ion doped in LNMO increase the lattice parameter of the material and can effectively inhibit the formation of rock-salt phase. Similarly, the excess of lithium doped into LNMO will also expand the lattice of the material; however, it also increased the formation of rock-salt phase, which hinders the diffusion of lithium ions. From the FT-IR spectroscopy, it can be seen that both of chlorine-doped and lithium-excess LNMO has mainly disordered phase with the space group of Fd3 ̅m at the 900oC sintering temperature. However, by comparing the ratio of the 586/624 bands, it can be found that the degree of ordering increase with the amount of chlorine doping. On the contrary, the excess of lithium would reduce the ordering of the transition metals in the crystal.
Moreover, it was found that the appropriate amount of chlorine doped in LNMO can improve the capacity and rate capability. It was also proved by dissolution test that chlorine doping can inhibit the dissolution of transition metal ions, which can reduce the chance of electrolyte oxidative decomposition and also improve the coulombic efficiency and retain better cycle life at high temperature. However, the excess of lithium doping in LNMO result in worse electrochemical performance, which was due to the formation of more inactive secondary phase and blocked the diffusion path of lithium ions.

摘要 V
Abstract VII
目錄 IX
表目錄 XII
圖目錄 XIII
第一章 研究背景與動機 1
第二章 文獻探討 5
2-1 LiNi0.5Mn1.5O4的晶體化學 5
2-2 LiNi0.5Mn1.5O4 的老化機制 12
2-3 提升LiNi0.5Mn1.5O4 性能的方法 17
2-3-1 電解液修飾 17
2-3-2 表面塗層 27
2-3-3 離子摻雜 30
第三章 研究方法 38
3-1 LiNi0.5Mn1.5O4 粉末製備 38
3-2 粉末特性分析 40
3-2-1 化學劑量分析 (ICP-OES) 40
3-2-2 粒徑分析 (PSA) 40
3-3-3 表面形貌分析（SEM） 41
3-3 結晶結構分析 42
3-3-1 X光繞射分析 (XRD) 42
3-3-2傅立葉轉換紅外光譜分析 (FT-IR) 42
3-4電池製備與測試 43
3-5溶出實驗 45
第四章 結果與討論 46
4-1氯摻雜對 LiNi0.5Mn1.5O4 特性之影響 46
4-1-1氯摻雜 LiNi0.5Mn1.5O4-xCly 之粉末特性分析 46
4-1-2氯摻雜 LiNi0.5Mn1.5O4-xCly 之結晶結構分析 55
4-1-3氯摻雜 LiNi0.5Mn1.5O4-xCly 之電化學特性 60
4-1-4溶出實驗 68
4-2氯摻雜配合鋰過量對 LiNi0.5Mn1.5O4 特性之影響 70
4-2-1氯摻雜配合鋰過量 Li1+zNi0.5Mn1.5O4-xCly 之粉末特性分析 70
4-2-2氯摻雜配合鋰過量Li1+zNi0.5Mn1.5O4-xCly之結晶結構分析 79
4-2-3氯摻雜配合鋰過量 Li1+zNi0.5Mn1.5O4-xCly 之電化學特性 83
第五章 結論 85
第六章 附錄 87
文獻探討 95

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