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研究生： 鍾玟雅
Chung, Wen-Ya
論文名稱： 矽碳複合材料應用於鋰離子電池負極材料之研究
Si / C composite as anode material for lithium ion batteries
指導教授： 黃肇瑞
Huang, Jow-Lay
共同指導教授: 張家欽
Chang, Chia-Chin
學位類別： 碩士
Master
系所名稱： 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年： 2019
畢業學年度： 107
語文別： 中文
論文頁數： 108
中文關鍵詞： 行星式球磨法 、熱處理 、矽 、SiOx 、SiOC 、碳氫樹脂 、矽碳複合材料 、負極材料 、鋰離子電池
外文關鍵詞： planetary ball-milling, heat treatment, silicon, SiOx, SiOC, hydrocarbon resin, Si/C composite, anode material, lithium ion batteries
相關次數： 點閱：144  下載：0 
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    • 本研究以碳氫樹脂為碳材前驅物製備矽碳複合材料，期望透過碳材導電性佳、機械強度高且表面SEI膜較為穩定的優點，以減緩矽材在充放電過程中體積膨脹收縮所帶來的效應，並避免矽直接與電解液接觸形成不穩定SEI膜以及防止矽之間於合金/去合金化反應後發生凝聚現象，另外矽的理論電容量高(3580 mAh/g)可以補足石墨理論電容量較低(372 mAh/g)的問題，兩種材料之間達到互補的作用以發展矽碳複合材料成為未來極具潛力的鋰離子電池負極材料。
    製備矽碳複合材料的方法很多種，本研究選用操作簡易、低成本、可大量製造且對環境友善的行星式球磨法搭配熱處理階段成功製備出矽碳複合材料，研究中主要探討熱處理溫度的變化對矽碳複合材料之影響，藉由活性材料特性分析以及電化學性能分析深入探討，而本研究更進一步改變矽碳複合材料中碳氫樹脂與矽粉之比例。
    本研究製備出以碳為基底作為骨架而奈米晶/非晶矽鑲嵌於其中的矽碳複合材料，並成功改善純矽材前幾圈電容量衰退問題。實驗中隨著熱處理溫度升高使得部分矽氧化程度提升並在矽與碳界面生成Silicon oxycarbide ( SiOC )加強矽碳之間的連結性。矽氧化物( SiOx )以及SiOC材料在充放電過程中會產生不可逆電容，然而生成的不可逆物質在接下來的反應過程中扮演良好的緩衝物，加上SiOx與SiOC材料本身鋰化/去鋰化反應時體積膨脹率小於純矽材，對複合材料結構影響較小，因此本研究成功製備出具有極佳電池循環穩定性的矽碳複合材料，同時兼具高電容量以及快速充放電的能力。

    We successfully synthesize the Si / C composites via a simple planetary ball-milling and heat treatment without high cost and risk of environment pollutions. This study shows that annealing temperature significantly affect oxidation degree and crystallite size of silicon as well as the formation of carbon buffer matrix in Si / C composites. The observed electrochemical performance of CPC / Si composite which was heated to 900 ℃ shows improved capacity (1702 mAh / g for first cycle charge) and good cycling ability ( 1340 mAh / g with 102 % retention after 100 cycles.). Thus, Si / C composites as anode material performs better electrochemical properties.

    中文摘要 I Extended abstract II 致謝 XI 總目錄 XIII 圖目錄 XVI 表目錄 XXIII 第一章 緒論 1 1.1 前言 1 1.2 研究動機與目的 1 第二章 文獻回顧 3 2.1 鋰離子電池發展與應用 3 2.2 鋰離子電池組成與工作原鋰 6 2.3 鋰離子電池負極材料介紹 9 2.3.1 碳負極材料 10 2.3.2 矽負極材料 11 2.3.3 金屬及過渡金屬氧化物負極材料 13 2.4 矽基負極材料的問題 14 2.4.1 活性材料崩解 15 2.4.2 固態電解質界面的形成 16 2.5 矽基負極材料的改善 18 2.5.1 材料尺寸與形貌之改變 18 2.5.2 矽氧化物作為負極材料 21 2.5.3 矽基合金與複合材料 25 2.6 矽碳複合材料應用於負極材料之研究近況 31 2.6.1 矽碳複合材料 31 2.6.2 製備方法與其性能 32 第三章 研究方法與實驗步驟 42 3.1 實驗材料 42 3.2 實驗設備 42 3.3 實驗設計與架構 42 3.4 活性材料的製備 43 3.4.1 ( 1:1 ) CPC / Si 複合材料 43 3.4.2 ( 1:3 ) CPC / Si 複合材料 45 3.5 材料鑑定分析 46 3.5.1 X-ray繞射分析儀 (X-ray diffraction spectrometer : XRD) 46 3.5.2 電子能譜化學分析儀 (Electron Spectroscopy for Chemical Analysis: ESCA) 47 3.5.3 拉曼光譜分析儀 (Raman spectroscopy: Raman) 48 3.5.4 傅立葉轉換紅外線光譜儀 (Fourier transform Infrared spectrometer : FTIR) 49 3.5.5 高解析場發射掃描式電子顯微鏡 (High resolution field emission scanning electron microscopy: FE-SEM) 49 3.5.6 高解析分析電子顯微鏡 (Ultrahigh Resolution Analytical Electron Spectroscopy: HR-AEM) 51 3.5.7 熱重分析儀 (Thermogravimetric analysis, TGA) 52 3.6 鈕扣型半電池組裝及性質測試 52 3.6.1 極片製作 53 3.6.2 電池組裝 53 3.6.3 半電池充放電測試 54 3.6.4 循環伏安法測試 55 3.6.5 交流阻抗測試 55 第四章 結果與討論 60 4.1 活性材料特性分析 60 4.1.1 XRD定性分析 60 4.1.2 Raman分析碳原子結構變化 63 4.1.3 FTIR官能基分析 65 4.1.4 ESCA分析鍵結能貢獻與變化 67 4.1.5 SEM分析表面形貌與顯微結構 76 4.1.6 TEM分析表面形貌與顯微結構 78 4.1.7 TGA矽碳重量比分析 81 4.2 電化學性能分析 83 4.2.1 電池化成行為分析 83 4.2.2 循環壽命充放電測試 87 4.2.3 不同充放電速率測試(C-rate) 93 4.2.4 循環伏安法分析 96 4.2.5 交流阻抗分析測試 99 第五章 結論 100 參考文獻 102

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