近年來，由於電動車市場之崛起與多功能可攜式電子產品之大幅進展，鋰離子電池的性能和需求與日俱增。其中，正極材料之發展尤其為一大關鍵，而高安全性、高輸出功率，與高能量密度電池皆為現今正極材料之必要條件與主流開發方向。因此，本研究針對高伏尖晶石之LiNi0.5Mn1.5O4-ϭ與富鋰層狀結構之xLi2MnO3·yLiNiaMnbO2等正極材料進行深入探討。
於尖晶石LiNi0.5Mn1.5O4開發方面，此博士論文延續本人之碩士期間的成果，探討晶格氧非計量比與粉體顆粒大小對於其電化學性能之影響，並針對高/低溫性能與對應之鋰離子擴散係數作詳細之探討，發現較高的氧非計量比與較小的顆粒大小具有較好的低溫性能與快速充放電能力，但在長圈數的高溫循環下卻會有顯著的電容量損耗，歸因於較高的錳溶出現象所導致。進一步研究指出，可藉由調整充放電電壓高於4 V來抑制此不良反應。另外，使用電化學阻抗量測並結合循環伏安分析法，證明LiNi0.5Mn1.5O4-ϭ之鋰離子擴散係數隨操作溫度呈指數變化，且不同充放電電位對其傳輸性能有劇烈影響，並發現操作溫度約為300K為本材料之鋰離子傳輸能力的關鍵，其牽涉Li/ LiNi0.5Mn1.5O4-ϭ系統中活化能的轉換。本研究亦開發出新型合成正極材料方法，可大幅提升尖晶石材料之粉體結晶性並增進快速充放電性能。
於富鋰層狀之正極材料開發方面，本研究首先針對其複雜結構與元素組成著手，經由系統性的分析與實驗探討，找出最適化複合成分為0.5Li2MnO3·0.5LiNi0.5Mn0.5O2，其具有完好的結晶性且無任何雜相殘留。本研究藉由引進有機溶劑製程法，可進一步控制粉體之合成形貌，製備出具有類似花狀之細微結構，此外，本製程亦可大幅抑制粉體表面碳酸鋰的覆蓋量，避免對富鋰正極材料之充放電性能造成負面影響，與傳統製程之顆粒狀粉體比較，發現前者具有較優異之電化學性能，在高速率放電下還可維持高電容量輸出，歸功於較低的藉面阻抗與較高的鋰離子擴散係數。
最後，本研究開發出新型之高分子氟化法，藉由前述有機溶劑製程方式，可一次性的製備出複合型正極粉體材料，其結合高伏尖晶石LiNi0.5Mn1.5O4-ϭ與富鋰層狀正極材料xLi2MnO3·yLiNiaMnbO2，目標為汲取前者之快速充放電與後者之高電容量等優點，可望進一步增進電池整體之功率輸出與能量密度。本技術相較其他合成方法相對簡易、快速、低耗能、降低成本，並具有可控制粉體形貌之優勢，此外，還可有效地達成更優異的電性表現，預期可應用於未來高功能性之鋰離子電池中。

Growing universal demands for alternative fuels and renewable energy sources have simulated the advancement of lithium-ion batteries, especially for the development of EVs. Breakthroughs in cathode materials are of the most demand to reach high power and energy density for future Li-ion batteries. The electrochemical performance depends on the morphological and compositional characteristics of the electrode materials, which could be optimized through controlling a variety of synthetic parameters. For future EVs usage, manganese based oxides are considered the most appreciable cathode materials with low cost and environmental benefits, yet still meet great challenges for pursuing high performances in Li-ion batteries. This dissertation aims to investigate ways to improve the rate capability of manganese based cathodes with three different structures: spinel, layered, and mixed spinel-layered phases.
Chapter 1 provides a history of lithium ion batteries, introduces some generalities and basic knowledge for electrochemical storages. Then, given an overview of the prototype cathode materials and its derivatives. It finally concluded that low cost and environmental-friendly manganese based oxides are much preferable for future EVs usage.
Chapter 2 gives a comprehensive literature review for three types of manganese based positive materials: high voltage spinel LiNi0.5Mn1.5O4-ϭ, high capacity Li-rich layered oxides yLi2MnO3∙xLiNiaMnbO2, and novel spinel-layered composites. The corresponded critical issues and main challenges are thoughtfully discussed. The aim of this study is also given in the end of this chapter, which is projected to pursuit high rate capability of cathode materials for achieving high power densities in lithium ion batteries.
Chapter 3 describes the synthetic processes used in this dissertation for obtaining subjected cathode materials. Various analytic methods and operation parameters are provided for identifying as-fabricated positive electrodes. Here, three evolutionary type of manganese based oxides with spinel, layered and spinel-layered mixed structures are designed, in which each material system is prepared via its corresponded fabrication method explained in each chapter.
Chapter 4 and 5 are devoted to the development of high voltage spinel LiNi0.5Mn1.5O4-ϭ cathode materials. The research in chapter 4 is a straight continuation of my M.S. thesis. Two key controlling factors, oxygen non-stoichiometry and particle sizes, are intensively explored for high voltage spinel cathodes and represented significant influences on electrochemical properties. In a detail examination, the profound correlations are found in these two factors associating to temperature durability of spinel cathodes. The EIS and CV techniques are proven very useful for studying the dependences of Li-ion diffusivity and the activation energy in electrochemical system of Li/ LiNi0.5Mn1.5O4-ϭ during temperature changes. A solvent-controlled co-precipitation method was introduced in chapter 5 for preparing a purified spinel cathode material with excellent rate performances. It reveals a well-dispersity and easy incorporation of various polymeric additives, which further contributes to my following research works.
Chapter 6 presents the evolution of complex composition and the architecture control of Li-rich layered oxides (LLOs). Based on theoretical and experimental investigations, the attainable compositions of LLOs were systematic evaluated. It finally concluded a most preferable composition of LLOs cathode material 0.5Li2MnO3∙0.5LiNi0.5Mn0.5O2 with high-crystallinity and without any undesired impurities. Moreover, the morphologically-tailored LLOs was successfully achieved via the inspiration of solvent-controlled synthetic method in chapter 5. It is favorable for accomplishing a good rate capability at relative high discharging rates.
Chapter 7 focuses on the development of spinel-layered composites (LLS) as a novel hybrid cathode material for lithium ion battery. A new strategy for achieving LLS material is implemented via particular fluoridations. The approach for evaluating relative spinel phases and the underlying mechanism of layer to spinel transformation is carefully addressed. In the end of this chapter, all of as-fabricated cathodes in this dissertation are compared with their rate capability at room temperature. As a result, a superior electrochemical performances of LLS cathodes are clearly highlighted. It successfully combines the high capacity Li-rich layered yLi2MnO3∙xLiNiaMnbO2 with the high voltage spinel LiNi0.5Mn1.5O4-ϭ to accomplish a complex composite cathode material with a generalized formula “yLi2MnO3∙xLiNiaMnbO2∙yLiNi0.5Mn1.5O4-ϭ”. It is greatly expected for the potential usage of high performance lithium ion batteries in future HEV/EVs.

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