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研究生： 陳慧蓮
Chen, Huei-Lian
論文名稱： 氧化矽奈米管與鎳鈷硫化物奈米片陣列應用於鋰離子電池負極之研究
Fabrications of SiOx Nanotube and Nickel Cobalt Sulfide Based Nanosheet Arrays as Negative Electrodes for Lithium Ion Batteries
指導教授： 吳季珍
Wu, Jih-Jen
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2018
畢業學年度： 106
語文別： 中文
論文頁數： 120
中文關鍵詞： 鋰離子電池 、負極 、無黏結劑電極 、氧化矽 、奈米管 、鎳鈷硫化物 、奈米片
外文關鍵詞： Lithium ion batteries, anode, binder-free electrode, SiOx, nanotube, NiCo2S4, nanosheet
相關次數： 點閱：65  下載：1 
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    • 本研究分別於碳布與發泡鎳上製備無黏結劑之氧化矽奈米管陣列與鎳鈷硫化物奈米片陣列電極，並探討其作為鋰離子電池負極之電化學特性。第一部分先利用化學浴法於碳布上成長氧化鋅奈米線陣列模板，繼以兩步驟溶膠凝膠法沉積氧化矽層於氧化鋅奈米線表面後，再以鹽酸水溶液去除氧化鋅奈米線，成功製備出氧化矽奈米管陣列，並應用於鋰離子電池之無黏結劑負極。由穿透式電子顯微鏡(TEM)分析得知，氧化矽奈米管之管壁厚度為 11 nm，而由TEM-EDS分析得知其矽氧比約為36:64。氧化矽奈米管陣列在200 mA/g的充放電速率下，具有1782 mAh/g之起始放電電容量，其起始庫倫效率可達91.1%。經200次循環後仍有1472 mAh/g的可逆放電電容量，電容量維持率為82.6%。而在2000 mA/g的充放電速率下，具有1457 mAh/g之起始放電電容量，其起始庫倫效率可達90.7%。經200次循環後仍有621 mAh/g的可逆放電電容量，電容量維持率為42.6%。由TEM分析經2000 mA/g下充放電循環400次後之電極，得知充放電循環造成之體積變化會使氧化矽奈米管之內徑變小，外徑增大，管壁厚度增加至16 nm，但仍可維持中空管狀結構，顯示經充放電循環後之電極結構並無崩解。本研究第二部份，則是利用化學浴法於發泡鎳上成長鎳鈷硫化物奈米片陣列，並應用於鋰離子電池之無黏結劑負極。由拉曼圖譜及X光繞射圖譜分析得知此奈米片陣列同時有鎳鈷硫化合物及鎳硫化合物存在，而由X光光電子能譜可得知其鎳鈷比約為56:44。此鎳鈷硫化物奈米片陣列電極在200 mA/g的充放電速率下，具有2353 mAh/g之起始放電電容量，其起始庫倫效率可達84.1%。經100次循環後仍有2195 mAh/g的可逆放電電容量，電容量維持率為93.3%。由上述可知，本研究成功製備出最適化之無黏結劑氧化矽奈米管陣列與鎳鈷硫化物奈米片陣列電極，應用於鋰離子電池負極時有良好且穩定之電化學性能表現。

    In this work, SiOx nanotube arrays have been successfully prepared by first coating ZnO nanowire templates on the surface of carbon cloth, followed by 2-step sol-gel synthesis and hydrochloric acid etching. When evaluated directly as binder-free anode for lithium-ion batteries, the resultant SiOx nanotube arrays electrodes exhibit excellent lithium storage performance with an improved cycle-life performance (approximate 17.4% capacity loss after 200 cycles at 200 mA g −1 with a capacity retention of 1472 mAh g−1 at the 200th cycle), and better rate performance (a reversible capability of 1476, 1375, 1147, 942, and 779 mA h g−1 at 200, 500, 1000, 2000, and 3000 mA g −1, respectively). The remarkably improved electrochemical performances could be attributed to following reasons. First, the conductive carbon cloth substrate offers fast electron transport. Besides, the nanotube structure of SiOx releases the stress of volume expansion, leading to a remarkably improved electrochemical performance. This novel composite electrode also holds the promising use in flexible LIBs.
    In another part, we have successfully developed binder-free NiCo2S4 based nanosheet arrays by directly growing the active material on Nickel foam in 1-step chemical bath deposition. Compared to the film electrode, the nanosheet electrode exhibited a better capacity and cycle-stability. The self-supported NiCo2S4 based nanosheet arrays exhibited a remarkable rate performance (a reversible discharge capacity of 2255, 1612, 1358, 1171, and 1049 mAh g −1 at 200, 500, 1000, 2000 and 3000 mA g −1, respectively) as well as remarkable cycling performance (approximate 6.7% capacity loss after 100 cycles at 200 mA g −1 with a capacity retention of 2195 mAh g −1 at the 100th cycle). The remarkably improved electrochemical performances could be attributed to following reasons. First, the conductive Ni foam substrate offers fast electron transport and high specific surface area. Besides, the nanosheet structure of Nickel Cobalt Sulfide releases the stress of volume expansion, leading to a remarkably improved electrochemical performance.

    摘要 I 誌謝 VII 目錄 IX 表目錄 XII 圖目錄 XIII 第一章 緒論 1 1.1 前言 1 1.2 鋰離子電池 3 1.2.1 發展與介紹 3 1.2.2 鋰離子電池工作原理 4 1.2.3 負極材料 6 1.2.4 無黏結劑電極(binder-free electrodes) 10 1.3 研究動機 11 第二章 文獻回顧 13 2.1 氧化矽於鋰離子電池負極材料之應用 13 2.1.1 二氧化矽之性質、結構及應用 13 2.1.2 氧化矽(SiOx)之性質、結構及應用 14 2.1.3 以溶膠凝膠法(Sol-gel method)成長氧化矽 16 2.1.4 氧化矽於鋰離子電池負極之應用 18 2.2 鎳鈷硫化物於鋰離子負極材料之應用 27 2.2.1 鎳鈷硫化物之性質及應用 27 2.2.2 鎳鈷硫化物之製備方法 28 2.2.3 硫化鎳(Nickel Sulfide)於鋰離子電池電極之應用 32 2.2.4 鎳鈷硫化物於鋰離子電池負極之應用 37 第三章 實驗方法 43 3.1 研究材料 43 3.1.1 製備氧化鋅奈米線陣列之材料 43 3.1.2 製備氧化矽奈米管陣列之材料 43 3.1.3 製備鎳鈷硫化物奈米片陣列之材料 44 3.1.4 組裝鈕扣型電池之材料 44 3.2 製備氧化矽奈米管陣列於碳布之實驗流程 46 3.2.1 基板清洗 47 3.2.2 成長氧化鋅晶種層 47 3.2.3 成長氧化鋅奈米線陣列 47 3.2.4 以超音波震盪輔助製備氧化鋅-氧化矽核-殼奈米線陣列 48 3.2.5 以浸鍍法輔助製備氧化鋅-氧化矽核-殼奈米線陣列 48 3.2.6 以酸蝕刻製備氧化矽奈米管陣列 48 3.2.7 組裝鈕扣型電池 48 3.3 製備鎳鈷硫化物奈米片陣列於發泡鎳之實驗流程 50 3.3.1 以化學浴法成長鎳鈷硫化物奈米片陣列 51 3.3.2 組裝鈕扣型電池 51 3.4 分析與鑑定 52 3.4.1 掃描式電子顯微鏡 52 3.4.2 穿透式電子顯微鏡 54 3.4.3 X光繞射儀 55 3.4.4 拉曼光譜分析儀 57 3.4.5 X光光電子能譜儀 58 3.4.6 電池充放電能力測試 59 3.4.7 循環伏安法 60 3.4.8 電化學阻抗頻譜分析 61 第四章 氧化矽奈米管陣列應用於鋰離子電池負極之研究 64 4.1 以碳布為基板製備氧化矽奈米管陣列 64 4.1.1 成長氧化鋅奈米線陣列模板 64 4.1.2 以氧化鋅奈米線陣列為模板製備氧化矽奈米管陣列 65 4.1.3 氧化矽奈米管陣列之分析及鑑定 74 4.2 氧化矽奈米管陣列應用於鋰離子電池負極 77 4.2.1 循環伏安法測試(Cyclic Voltammetry) 77 4.2.2 循環壽命與變電流穩定度測試 78 4.2.3 氧化矽奈米管陣列經充放電循環後之分析與鑑定 84 4.2.4 氧化矽奈米管陣列經充放電循環後之交流阻抗分析 86 第五章 鎳鈷硫化物奈米片陣列應用於鋰離子電池負極之研究 89 5.1 以發泡鎳為基板製備鎳鈷硫化物奈米片陣列 89 5.1.1 反應物濃度對製備鎳鈷硫化物奈米片陣列之影響 89 5.1.2 反應時間對製備鎳鈷硫化物奈米片陣列之影響 90 5.2 鎳鈷硫化物奈米片陣列之分析及鑑定 94 5.3 鎳鈷硫化物奈米片陣列應用於鋰離子電池負極 99 5.3.1 循環伏安法測試(Cyclic Voltammetry) 99 5.3.2 循環壽命與變電流穩定度測試測試 100 5.3.3 鎳鈷硫化物奈米片陣列經充放電循環之分析與鑑定 104 5.3.4 鎳鈷硫化物奈米片陣列經充放電循環後之交流阻抗分析 105 第六章 結論 108 第七章　參考文獻 111

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