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研究生： Arif Cahyo Imawan
Arif Cahyo Imawan
論文名稱： 通過原子轉移自由基聚合技術將矽表面接枝聚丙烯酸和聚β-羧乙基丙烯酸酯並應用於鋰離子電池的負極材料
The Grafting of the Polyacrylic acid and Poly β-carboxyethyl acrylate on the Silicon Surface Via Atomic Transfer Radical Polymerization (ATRP) Technique and Their Application as Anode Material of Lithium Ion Battery
指導教授： 王復民
Fu-Ming Wang
口試委員: 郭俞麟
Yu-Lin Kuo
王丞浩
Chen-Hao Chen
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： 2020
畢業學年度： 108
語文別： 英文
論文頁數： 110
中文關鍵詞： 聚丙烯酸 、β-羧乙基丙烯酸酯 、矽 、原子轉移自由基反應 、鋰離子電池
外文關鍵詞： acrylic acid, β-carboxyethyl acrylate, silicon, atomic transfer radical polymerization, Li ion battery
相關次數： 點閱：226  下載：0 
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    • 聚丙烯酸(AA)與β-羧乙基丙烯酸酯(CEA)以原子轉移自由基過程的技術接枝在矽的表面上以及其技術應用於鋰離子電池的負極材料已有許多發表。本研究主要是著重在AA與CEA的高分子聚合物接枝於矽的表面，分析這些接枝的高分子聚合物在矽負極的影響，以及黏合劑與矽的顆粒大小所造成的影響。
    為了接枝AA與CEA至矽的表面，本研究首先將矽使用氟化氫蝕刻矽的表面，接著ATRP的起始劑會透過氫矽化反應接枝在矽的表面，而ATRP的最後一步驟會以Cu(I)-Bipy催化並完成反應。為了分析電池性能，本研究使用充放電分析、循環伏安法以及電話學阻抗分析等技術。羧甲基纖維素(CMC)以及聚二氟亞乙烯(PVdf)作為本研究的黏著劑，同時，我們也將探討黏著劑對於矽的顆粒大小在微米以及奈米等級之影響。
    根據研究結果，我們認為CMC黏著劑與PVdf黏著劑相比，有較好的穩定性。此外，當矽的顆粒微奈米等級時，也有較好的循環表現。當AA接枝於矽負極時，會有增加電容率，但在長時間的循環下缺乏穩定度。而CEA接枝於矽負極時，除了可以增加電容率外，亦可有高穩定性。綜合本研究的所有結果，矽-CEA於0.1奈米時會是最佳的電極材料因為矽-CEA可以在200圈充放電後電容為1188 mAh g-1且每一圈僅減少0.27%的電容率。

    The grafting of the poly acrylic acid (AA) and poly β-carboxyethyl acrylate (CEA) on the silicon surface via atomic transfer radical polymerization (ATRP) technique and their application as anode material of lithium ion battery has been conducted. This research’s purpose is to graft the AA and CEA polymer on the surface of the silicon and to analysis the effect of this grafted polymers on the silicon anode performance. Moreover, the effect of the binder and silicon size have been carried out.
    To graft the AA and CEA, the silicon was etched by using the HF. Then, the ATRP initiator was attached on the silicon surface via hydrosilylation reaction. The last step was ATRP reaction catalyzed by Cu(I)-Bipy. To analysis the battery performance, the charge-discharge, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were used. Carboxymethyl cellulose (CMC) and polyvinylidene fluoride (PVdF) binders were used to analysis the effect of the binder, while silicon with macro (⁓325 nm) and nano (<100 nm) were used to analysis the effect of the silicon sizes.
    The result confirmed that the CMC binder had better stability performance compared with PVdF binder. Moreover, the silicon with nano size gave a better long cycle performance compared with macro size. The presence of AA on the silicon anode enhanced the capacity, but it had poor stability during long cycle. While, the presence of the CEA enhanced the capacity and gave a higher stability. From the analysis, Si-CEA0.1 nano was the best electrode among the other since Si-CEA was able to deliver 1188 mAh g-1 after 200 cycles with capacity loss 0.27% per cycle.

    Table of Content Cover I Master’s Thesis Recommendation Form II Qualification Form by Master’s Degree Examination Commitee III ABSTRACT IV 摘要 V Acknowledgment VI Table of Content VII List of Figure IX CHAPTER I INTRODUCTION 1 I.1. Background 1 I.2. Problem Formulation 4 I.3. Research Purposes 5 CHAPTER II LITERATURE REVIEW 6 II.1. Lithium-Ion Battery Components 6 II.1.1. Cathode 6 II.1.2 Anode 9 II.1.3 Electrolyte 13 II.1.4 Separator 14 II.2. Silicon anode and modified silicon anode 16 II.2.1 Silicon anode 16 II.2.2 Fundamental Challenges and Solutions 16 II.2.3 Modified silicon anode 27 II.3 The Modification of Silicon Surface with Polymer Via ATRP Techniques 28 II.3.1. Silicon etching and H-terminated silicon 28 II.3.2. Hydrosilylation reaction 30 II.3.3. Free radical and ATRP polymerizations process 33 II.3.4 Acrylic Acid (AA) and 2-carboxyethyl acrylate (CEA) 42 CHAPTER III RESEARCH METHODOLOGY 45 III.1 Research Design 45 III.2. Materials 49 III.3. Equipments 49 III.4. Experimental Procedure 50 III.4.1. The synthesis of the silicon polymer via ATRP technique 50 III.4.2. The electrode fabrication 51 III.4.3. The coin cell assembling 51 III.4.4. Battery performance 52 CHAPTER IV RESULT AND DISCUSSION 53 IV.1. Silicon Surface Modification with Polymer Synthesized Via Atomic Transfer Radical Polymerization (ATRP) Technique 54 IV.1.1. The etching and hydrosilylation processes of the silicon 55 IV.1.2. The polymer growth on the surface of the silicon via atomic transfer radical polymerization (ATRP) reaction 56 IV.2. The Electrode Slurry and Coating 68 IV.3. Battery Performance 73 IV.3.1 The effect of the binder types 73 IV.3.2 The effect of the polymer types 80 IV.3.3 The effect of the silicon size 91 CHAPTER V CONCLUSION 100 References 102

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