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研究生： ARIONO VERDIANTO
ARIONO VERDIANTO
論文名稱： 氟化馬來醯亞胺異構物電解液添加劑用於鋰離子電池矽陽極性能探討之研究
The Investigation of Fluorinated Maleimide Isomers as the Electrolyte Additive for the Silicon Anode in Lithium-Ion Battery
指導教授： 王 復 民
Wang Fu-Ming
口試委員: 楊純誠
Chun-Chen Yang
王丞浩
Chen-Hao Wang
王 復 民
Fu-Ming Wang
學位類別： 碩士
Master
系所名稱： 應用科技學院 - 應用科技研究所
Graduate Institute of Applied Science and Technology
論文出版年： 2017
畢業學年度： 105
語文別： 英文
論文頁數： 121
中文關鍵詞： 矽 、固態電解質界面 、馬來醯亞胺添加劑 、鋰離子電池
外文關鍵詞： silicon, solid electrolyte interface, maleimide-based additive, lithium ion battery
相關次數： 點閱：365  下載：1 
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    • 矽為一非常有潛力的陽極材料因其超高的電容量(〜4200mAh/g)，比石墨作為陽極(〜372mAh/g)高出約十倍。然而，經過數次充放電循環後體積會大量膨脹> 300％。在這項研究中，我們觀察氟化異構物馬來醯亞胺的作用，用以抑制體積膨脹之缺點且延長電池的使用壽命。目前研究已經證明加入此種添加劑使用於矽材料作為負極的情況下對鋰離子電池循環性能具有顯著影響。透過具有更高的還原電位，氟化異構物馬來醯亞胺添加劑將比碳酸酯基電解液更減少SEI層的生成，且減少鹽類的分解量。由實驗結果可以確信馬來醯亞胺的還原在陽極表面提供更穩定的鈍化層，以防止在循環伏安法時發生寄生反應且馬來醯亞胺電解液添加劑正還原電位(〜2.4 V)比碳酸酯電解液(如EC:DEC)具有更大的正還原電位(〜1.5 V)。在研究中，碳酸酯電解液被認為是SEI形成的指標。本研究進行了深入的探討，特別是鋰離子電池添加劑對於SEI的形成的影響。而實驗採用交流阻抗（EIS）來分析關於鋰離子電池阻抗以及電池內阻的資訊。為了觀察表面形態的變化，我們也使用掃描電子顯微鏡（SEM）進行測試。 SEM提供了關於SEI型態變化的物理信息，同時為了分析SEI的組成，我們也進行了XPS測試。總體來說，與先前研究相比，使用添加劑在電解液上有著明顯的改善與優勢。

    Silicon is well known potential candidate as material for anode due to gravimetric energy capacity ~4200 mAh/g which is around ten times higher than graphite-based anode ~372 mAh/g but it is suffered from huge volume expansion >300% after several times of cycling. In this study, we trying to observe the fluorinated maleimide isomer effect for addressing this grievous in order to suppress the volume expansion and finally extend the life time of the batteries. This additive has been proved for having significant impact on lithium-ion battery cycling performance in the case of graphite used as negative electrode material. By having higher reduction potential, fluorinated maleimide isomer additive will reduce earlier than electrolyte components, the carbonate-based electrolyte, to form SEI layer and then reduce the amount of salt decomposition. It was believed that the reduction of maleimide provide more stable passivation layer on the surface of anode to prevent the parasitic reaction being happened. Cyclic voltammetry result depicts that maleimide-based electrolyte additive has more positive reduction potential ~2.4 V than carbonate-based electrolyte ~1.5 V such as EC: DEC which is assumed to be the indicator of SEI formation. A further study has been done to take an assessment of the additive impact on lithium-ion batteries especially for SEI formation. Electrical impedance spectroscopy (EIS) will give the information about impedance of lithium-ion batteries as well as the internal resistance of the batteries. To observe the surface morphology changing, we run scanning electron microscopy (SEM) test. SEM provides the information of the physical information of SEI regarding the morphology changing and to analyze the composition of SEI, XPS testing has been conducted. Overall, there is an improvement the adding of additive onto electrolyte compare to this system without the presence of additive.

    ABSTRACT IV 摘要 V ACKNOWLEDGEMENT VI TABLE OF CONTENTS VII LIST OF FIGURES X LIST OF TABLES XIII CHAPTER I 1 INTRODUCTION 1 1.1 Background 1 1.2 Problem Formulation 8 1.3 Research Purpose 9 CHAPTER II 10 LITERATURE REVIEW 10 2.1 Internal Structure of Lithium-ion Batteries 12 2.1.1 Cathode 12 2.1.1.1 Layered oxides 14 2.1.1.2 Spinels 14 2.1.1.3 Olivines 15 2.1.2 Anode 16 2.1.2.1 Carbon anodes 16 2.1.2.2 Alloying anodes 17 2.1.3 Electrolyte 20 2.1.3.1 Electrolyte solvents. 20 2.1.3.2 Salts 22 2.1.3.3 Additives of Electrolyte 25 2.1.4 Separator 27 2.2 Silicon Anode 30 2.2.1 Lithium-Silicon System 30 2.2.2 Silicon Volume Expansion 33 2.2.3 Electrolyte for Silicon Alloys 34 2.3 Solid Electrolyte Interface (SEI) 38 2.3.1 General Carbonate-based Electrolyte Reduction 39 2.3.2 The Formation SEI layer 43 2.3.3 SEI layer evolution 44 2.4 Maleimide-based Additive 45 CHAPTER III 49 RESEARCH METHODOLOGY 49 3.1 Research Design 50 3.2 Materials 51 3.3 Equipment 52 3.4 Experimental procedure 53 3.4.1 Synthesis of Fluorinated Maleimide Additive 53 3.4.2 Fabrication of SiNPs@CMC. 53 3.4.3 Electrolyte and Battery Preparation 54 3.5 Electrochemical testing 56 3.5.1 Cyclic voltammetry (CV) test 56 3.5.2 Charge discharge test 56 3.5.3 Electrochemical Impedance spectroscopy (EIS) test 57 3.6 SEI Layer Evaluation 57 3.6.1 Scanning Electron Microscopy (SEM EDX) test 57 3.6.2 X-Ray Photoelectron Spectroscopy (XPS) test 58 CHAPTER IV 59 SYNTHESIS MALEIMIDE BASED-ADDITIVE 59 4.1 Synthesis 59 4.1.1 Synthesis Procedure of MI-based Additive 61 4.1.1.1 Hydrogenation Part 61 4.1.1.2 Dehydration 62 4.2 Characterization 64 4.2.1 Mass Spectral 64 4.2.1 1-fluoro-ortho-phenylenediamine 64 4.2.1 2-fluoro-ortho-maleimide (Ortho) 64 4.2.2 FTIR-ATR characterization 67 4.3 Electrolyte Preparation 72 CHAPTER V 73 RESULT AND DISCUSSION 73 5.1 Electrochemical Analysis 73 5.1.1 Cyclic Voltammetry 73 5.1.2 Cycling Performance 78 5.1.3 Electrical Impedance Spectroscopy (EIS) Testing 82 5.2 Solid Electrolyte Interface (SEI) Evaluation 86 5.2.1 Scanning Electron Microscopy (SEM EDX) analysis 86 5.2.2 ex situ X-ray Photoelectron Spectroscopy (XPS) 89 CHAPTER VI 98 CONCLUSION 98 REFERENCES 100

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