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研究生： 曾偉良
Chen, Wai-Leong
論文名稱： 奈米碳片，鑽石，石墨烯與其複合薄膜在電化學與場發射上的應用
Carbon nanowall, diamond, graphene and related carbon composite films for electrochemical and field emission applications
指導教授： 曾永華
Tzeng, Yonhua
學位類別： 碩士
Master
系所名稱： 電機資訊學院 - 微電子工程研究所
Institute of Microelectronics
論文出版年： 2011
畢業學年度： 99
語文別： 中文
論文頁數： 206
中文關鍵詞： 石墨烯 、奈米碳片 、直流電漿化學氣相沉積法 、熱分解化學氣相沉積法
外文關鍵詞： Graphene, Carbon nanowalls, Direct-current PECVD, Thermal CVD
相關次數： 點閱：104  下載：4 
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    • 本實驗主要分成兩大部分，第一部分是以石墨烯製程為主，除了探討石墨烯的製程實驗與分析外，也進一步量測其電化學的特性。除此之外，我們也發展了一種石墨烯的轉移技術，在不使用PMMA下成功地把石墨烯薄膜大面積的從銅箔片轉移到任何基板上。第二部分是以奈米碳片的製程與應用為主，並且我們結合鑽石薄膜與奈米碳片製得幾種不同的複合材料，在電化學的應用上也取得不錯的成果。最後，我們以透射式電子顯微鏡進一步探討成長於矽基板上的奈米碳片，並且深入探討奈米碳片在矽基板上的成長機制。
    奈米碳片、石墨烯與鑽石等其他碳材料結構都是碳的同素異構物。雖然以化學沉積法成長鑽石薄膜的技術早在半個世紀前就已經開始發展，但因為成長速率的限制與鑽石單晶成長難以控制，合成鑽石的技術在近20年才開始蓬勃發展。自1985年 Fullence-C60被發現以來，碳材料的課題一直備受關注，因為C60的獨特特性使它能夠應用在不同領域上，也引起不少的研究學者投入了碳材料的研究領域。在1991年日本科學家飯島澄男偶然發現了奈米碳管 ，奈米碳管擁有特殊的電子傳導特性且具有類似鑽石的楊氏模數，因此引起許多科學家的關注。但是，奈米碳管為一維結構，在應用上有所侷限，所以許多科學家開始探討二維結構碳材料存在的可能性。2004年，英國曼徹斯特大學的A.K.Geim與K.S.Novoselov等研究團隊以膠帶剝落法取得二維的單層石墨烯薄膜，引起許多研究團隊紛紛投入了石墨烯的研究領域；2010年，A.K.Geim與K.S.Novoselov學者也以「二維特殊材料石墨烯進行突破性實驗」奪下了諾貝爾物理獎。目前半導體工業技術發展迅速，在積體電路元件設計上因尺寸縮小化的限制，造成許多發展上的瓶頸。然而，因為石墨烯的電子傳導速率快，而且僅為原子層的厚度，在未來工業應用上扮演著重要的角色。

    Carbon nanowalls (CNWs) with nano-meter sharp edges extending in a two-dimensional wall-like network and a large effective surface area are useful for many applications including high current density and low voltage electron emitters operating at room temperature. Diamond has high hardness, high thermal conductivity, chemical inertness, etc. and, therefore, many potential advantages of combining outstanding properties of diamond and those of carbon nanowalls to achieve excellent performance. We have fabricated CNWs using Direct Current (DC)-Plasma Enhanced Chemical Vapor Deposition (DC-PECVD) in gas mixtures of methane and hydrogen. Diamond was synthesized using Microwave Plasma Enhanced Chemical Vapor Deposition (MW-PECVD) and DC-PECVD processes also in gas mixtures of methane diluted by hydrogen with or without argon additive. Several carbon nanostructures including CNWs and diamond nanowalls (DNWs) as well as carbon nanowall-in-diamond(CNW-in-D), and carbon nanowall-on-diamond (CNW-on-D) composite structures have been synthesized. The synthesis processes, properties and applications of these carbon nanostructures as electron field emitters and electrochemical electrodes will be reported.
    HR-TEM examination of the interface between graphene and silicon shows that multi-layer graphene (002) planes are epitaxial on silicon (111) plane and surrounded by amorphous carbon. The lattice mismath is about 8% between these two planes. The stress is realesed by dislocations. We attribute the heteroepitaxial growth of graphene on silicon to the fact that the (100) silicon substrate is etched by hydrogen-rich plasma at the CNW growth temperature of 800-900C to form many (111) planes, which, in turn, result in many dangling bonds for reacting with C2 radicals to allow heteroepitaxial growth of graphene on silicon with dislocation at the interface to relax partial lattice mismatch. Raman spectra show signaficantly strong G and 2D band of graphene. The synthesis processes, properties and growth mechanism of this hetero-epitaxial multi-layer nano-graphene from plasma modified surfaces of silicon substrate will be reported
    A novel process for transferring thermal CVD single-layer graphene from copper foils to destination substrates and the characteristics of transferred graphene and its modified graphene after being subjected to hydrogenation in a remote microwave plasma in hydrogen are presented. Although graphene is mechanically very strong, considering its atomically thin structure, large-area single-layer graphene is practically very fragile especially during handling and transfer from one substrate to another. Handling of large-area free-standing graphene is even more challenging. Hydrogenation of graphene allows fine tuning of its electrical resistivity. Properties and applications of hydrogenated graphene transferred to destination substrates by a novel transfer process with minimum stress induced during handling are reported.

    中文摘要 ........................................... I 英文摘要(Abstract) ................................ II 致謝 ............................................. IV 總目錄 ............................................ VI 圖目錄 ............................................. X 表目錄 ........................................... XXV 第一章 緒論 ......................................... 1 1-1 石墨烯介紹 ...................................... 1 1-2 奈米碳片介紹 .................................... 3 第二章 石墨烯-文獻回顧 ................................ 6 2-1 石墨烯的製備方式 .................................. 6 2-1-1 剝離法 ......................................... 6 2-1-1-1 機械式剝離法 ...................................6 2-1-1-2 水溶液機械剝離法 ............................... 7 2-1-2 化學氣相沉積法 ................................... 9 2-1-2-1 碳化矽上磊晶成長法 .............................. 9 2-1-2-2 電漿輔助化學氣相沉積法 .................. 10 2-1-2-3 熱分解化學氣相沉積法 ........................ 11 2-1-3 石墨烯在金屬銥、鎳和銅上成長機制的差異與討論 ........... 12 2-1-3-1 石墨烯在金屬銥薄膜上的成長機制討論 ................ 12 2-1-3-2 石墨烯在金屬鎳薄膜上的成長機制討論 ................. 12 2-1-3-3 石墨烯在金屬銅薄膜上的成長機制討論 ................. 16 2-2 石墨烯的大面積成長與轉移 ..............................21 2-2-1 石墨烯大面積的成長與其製程方式 ..................... 22 2-2-2 石墨烯其轉移方式 .............................. 27 2-2-3 氧化還原法 .................................... 37 2-3 石墨烯的各種檢測方式 ................................ 40 2-3-1 光學顯微鏡 ..................................... 40 2-3-2 原子力顯微鏡 .................................43 2-3-3 透射式電子顯微鏡 ...................................44 2-3-4 拉曼光譜儀 ...................................... 51 第三章 奈米碳片-文獻回顧 .................................. 60 3-1 0D、2D、3D 系統 ................................... 60 3-2 奈米碳片的成長機制 ................................... 62 3-3 奈米碳片的成長方式 ................................... 69 3-3-1 微波電漿化學氣相沉積法 .............................. 70 3-3-2 電感耦合電漿增強式化學氣相沉積法 ..................... 73 3-3-3 熱燈絲化學氣相沉積法 ............................... 77 3-3-4 蒸鍍法 ...................................... 78 3-4 奈米碳片的拉曼光譜分析 ......................... 80 第四章 實驗儀器與製程步驟介紹 ........................... 82 4-1 製程儀器 ..................................... 82 4-1-1 直流電漿化學氣相沉積系統 ........................ 82 4-1-2 熱分解化學氣相沉積系統 ........................... 88 4-1-3 微波電漿化學氣相沉積系統 ....................... 91 4-2 分析與量測儀器 ................................. 92 4-2-1 原子力顯微鏡 .................................. 92 4-2-2 掃描式電子顯微鏡 ................................ 93 4-2-3 拉曼光譜儀 ...................................... 94 4-2-4 場發射量測系統 .................................. 95 4-2-5 電化學量測系統 ................................. 96 4-2-5-1 循環伏安法 ................................. 96 第五章 石墨烯-實驗分析與結果討論 ............................ 97 5-1 石墨烯 ..................................... 97 5-1-1 成長石墨烯的製程參數 ............................... 97 5-1-2 銅箔片對石墨烯薄膜成長製程的影響 .................... 102 5-1-3 石墨烯的轉移方式 .................................. 105 5-1-4 石墨烯薄膜電化學特性的量測 ......................... 119 5-2 石墨烷 ...................................... 122 5-2-1 Graphane 的製程與其拉曼光譜分析與電性量測 ........... 122 第六章 奈米碳片-實驗分析與結果討論 ....................... 126 6-1 奈米碳片的製程 .................................. 126 6-1-1 奈米碳片隨著成長時間不同的討論 ................ 126 6-1-2 奈米碳片成長過程中其電流與電壓不同的影響 .......... 134 6-1-3 奈米碳片成長過程中其甲烷氣體流量的影響 ..........142 6-1-4 奈米碳片與微米多晶鑽石複合薄膜 ................ 144 6-1-5 奈米碳片在奈米鑽石薄膜內的複合薄膜 ............ 155 6-1-6 奈米鑽石片 ................................... 162 6-1-7 奈米碳片在微米多晶鑽石薄膜上的複合薄膜 .............. 166 6-1-8 奈米碳片在鑽石薄膜/矽基板/氧化矽基板的電化學比較 ...... 173 6-1-9 奈米碳片在鑽石薄膜/基板的電化學的使用壽命討論 ........ 181 6-1-10 奈米碳片成長於等向性石墨基板上的電化學特性 ........ 186 6-2 奈米碳片成長在矽基板上的透射式電子顯微鏡分析 .......... 192 第七章 未來展望........................................ 197 7-1 冷壁反應爐成長石墨烯薄膜 ..........................197 7-2 石墨烷及石墨烯在不同閘極絕緣層材料下的場效電晶體特性 ..... 198 7-3 石墨烯與不同金屬接觸下的電性量測 .................... 199 參考文獻 ............................................. 200

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