本研究針對過量鋰層狀材料結構的變化，藉由臨場分析技術進行結構變化的分析，以獲得在不同狀態下材料結構變化的趨勢。經臨場X光繞射分析得知，當充電至>4.4V時可發現異相結構特徵峰的產生，顯示材料充電至高電壓區段時，因結構的不穩定及氧缺陷的產生，將造成結構的轉變，而當放電至2V時可發現異質結構繞射峰(Li1-xMn2O4(400))的產生，其可能是Mn還原所造成的結構轉變。另外由臨場拉曼檢測分析得知，當過充電至5V時，將提升過渡金屬的遷移及氧空缺的生成，造成表面結構應力的增加及結構的局部扭曲，進而導致材料表面尖晶狀異質結構區域的增加。而這些尖晶狀異質結構，應為極化現象發生的主因。
自身終止高分歧寡聚物(self terminated oligomers with hyper branched architecture, STOBA)，近年來被添加於鋰離子電池中，以提供高度安全保護機制，防止熱失控產生爆炸的現象。其反應機制包含互相競爭之麥可加成反應(Michael addition reaction)與自由基聚合反應(Free radical polymerizations reaction)。本研究主要針對不同Barbituric acid (BTA、1,3-dimethylbarbituric acid、5,5-dimethylbarbituric acid)單體與N,N’-bismaleimide-4,4’-diphenylmethane (BMI)合成之STOBA，於熱效應及電壓效應下，藉由臨場拉曼增強光譜分析其反應機制的趨勢。實驗結果可知，BTA與1,3BTA所合成的STOBA其特徵峰訊號隨溫度的升高而下降，顯示材料逐漸構築成綿密的立體保護網。然而5,5BTA所合成的STOBA反應性較慢與BMI的聚合程度低，由此可知C=C雙鍵容易與C-H鍵反應形成完整的保護膜，但不易與N-H鍵上的氫反應，因此需要較高的溫度以及較長的時間才能有聚合交聯的發生。

In this work, we focus on the observation of layered Lithium rich material structure by in-situ analysis technology during charge-discharge steps. From in-situ XRD analysis, the peaks for heterogeneous structure appear when charged over 4.4V. It means the structure of cathode material is unstable at high potential and due to the formation of oxygen vacancy which caused metal transition in the structure. When discharged to 2V, the structure also changed and the diffraction peak of (Li1-xMn2O4(400)) can be found from Mn reduction. After that, in-situ Raman spectrum analysis revealed that when cathode material over charged to 5V, the migration of transition metal and the formation of oxygen vacancy can be increased, resulting in the enhancement of surface stresses and local structure distortion. Furthermore it increased the spinel-like heterogeneous structure on material’s surface which supposed to be the main reason of polarization.
Self terminated oligomers with hyper branched architecture (STOBA) are added into Lithium ion battery to provide high safety protection mechanism and prevent thermal runaway explosion in recent years. The two major competitive reactions include Michael addition reaction and free radical polymerizations reaction. In this work, we studied STOBAs reaction mechanisms using different Barbituric acids (BTA, 1,3-dimethylbarbituric acid, 5,5-dimethylbarbituric) with N,N’-bismaleimide-4,4’-diphenylmethane (BMI) monomer under thermal treatment and potential treatment by in-situ SERS. Compared to the results, STOBAs’ vibration peaks decreased during the temperature change when using BTA and 1,3BTA with BMI. It reveals that STOBA gradually crosslinked and built a dense three-dimensional network protection film. However the polymerization of 5,5BTA with BMI is slow and hard to identify its molecular vibration change. Above all, C=C double bond is more likely to react with C-H bond to form the completely film while C=C double bond needs longer time or higher temperature to trigger the polymerization of STOBA in N-H bond.

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