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研究生:陳栢峰
研究生(外文):Bai Fong Chen
論文名稱:使用熱化學氣相沉積法低溫成長石墨烯及其特性探討
論文名稱(外文):Characterization and Synthesis Graphene by Thermal Chemical Vapor Deposition at Low Temperature
指導教授:陳密陳密引用關係
指導教授(外文):Mi Chen
口試委員:顧鴻壽張憲彰
口試日期:2013-06-14
學位類別:碩士
校院名稱:明新科技大學
系所名稱:化學工程與材料科技系碩士班
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2013
畢業學年度:101
語文別:中文
論文頁數:68
中文關鍵詞:石墨烯化學氣相沉積三階段加熱區低溫
外文關鍵詞:GrapheneLow TemperatureCVD3-stage heating
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石墨烯(Graphene)是碳原子以sp2鍵結成蜂巢晶格之平面薄片結構,其厚度只有一層碳原子厚,是目前最薄且最硬的奈米材料,也是一種透明且良好的導體。由於石墨烯具有獨特的結構與優異的物理特性,可應用於奈米電子元件、透明觸控螢幕、觸控面板、電容器、鋰電池、太陽能電池複合材料和儲氫材料等。石墨烯的製備方法主要有機械剝離法、加熱碳化矽法、氣相沉積法和化學氧化法等,其中以熱化學氣相沉積法最適合大量生產,因為其容易操作與設備構造簡單。但傳統之熱化學氣相沉積法製程溫度高(900~1100℃),高溫製程只適用高熔點材質之基板,再轉印於ITO玻璃基板上,或矽基板上,轉印增加製程成本、費時與有化學品殘留等問題。
本論文將以三階段加熱區之熱化學氣相沉積系統低溫成長石墨烯,本論文在不同基板(銅箔、二氧化矽)上低溫成長石墨烯,以常用之反應氣體,氫氣-甲烷-氬氣為製程氣體。第一、二段高溫區溫度設定950℃,以維持足夠之熱能分解碳氣體源甲烷,第二段中置入原始銅箔當作催化劑,將第三段之基板加熱區溫度區設定550℃,低溫成長石墨烯;對石墨烯之應用將可降低轉印之成本與製程時間。以二氧化矽為基板在高溫區或低溫區皆可成長石墨烯,但石墨烯缺陷高而品質低。結果顯示,以三段式化學氣相沉積法,可以在低溫區550℃成長高品質單層石墨烯,以及重複堆疊成長雙層、三層石墨烯,且成長所得石墨烯缺陷低而品質佳。本論文亦探討以H2-CH4為反應氣體,在銅蒸氣的氛圍下低溫成長石墨烯之反應機制。

Graphene is a one atom thick planar sheet of sp2 bonded carbon atoms that are packed in a honeycomb crystal lattice structure. Graphene is the thinnest and hardest nano-materials. Graphene is an important transparent conductive material with unique structure and excellent properties which has a wide range of applications in optics, optoelectronics, gas sensors, capacitor, touch panel, composite materials, solar cells, and hydrogen storage materials. Various methods have reported for the synthesis of graphene, which includes: mechanical exfoliation from HOPG, Epitaxial growth method, chemical oxidation method, and Chemical vapor deposition method. Thermal Chemical vapor deposition (CVD) has been employed large-area production due to the simple equipment and easy operation. However, graphene usually synthesize at relatively high temperature (900~1100℃) by a thermal CVD. Higher operation temperature is limited the substrate materials that need transfer process. It has time-consuming, chemical residue, and cost problems.
In this thesis, graphene was synthesized on various substrate (copper, SiO2) at low temperature by a thermal CVD using Ar-H2-CH4 gas mixture. The carbon source reactant CH4 was heated at high temperature (950℃) in the first and second heating zone, a copper foil put on second heating zone as a catalyst, and graphene was synthesized at low temperature (550℃) in the third heating zone. The results show that high quality single layer, bi-layer and tri-layer graphene were successful synthesized at low temperature zone by 3-stage heating zone thermal chemical vapor deposition system. The reaction mechanism and of graphene synthesis under H2-CH4 and copper vapor ambient at low temperature was also investigated in this study.

摘要 i
Abstract ii
誌謝 iii
目錄 iv
表目錄 vi
圖目錄 vii
第一章緒論 1
1.1前言 1
1.2 研究動機 2
第二章文獻回顧 4
2.1石墨烯之發現 4
2.2 石墨烯的結構 5
2.3 石墨烯之特性 7
2.4 石墨烯之製備方法 11
2.4.1 機械剝離法 12
2.4.3 碳化矽磊晶成長法 12
2.4.4 氧化還原法 13
2.4.2 化學氣相沉積法 14
第三章實驗方法與儀器 18
3.1 實驗流程圖 18
3.2 石墨烯之製備 19
3.2.1 改變氫氣流量對石墨烯成長之效應 19
3.2.2 改變甲烷流量對石墨烯成長之效應 22
3.2.3 持溫段改變氫氣流量成長石墨烯之探討 23
3.2.4 成長寡層石墨烯之特性分析 24
3.2.5 以二氧化矽為基板成長石墨烯 25
3.2.6 石墨烯之轉印 26
3.2.7 特性分析 27
3.3 儀器裝置 28
3.3.1 掃描式電子顯微鏡(Scanning Electron Microscopy, SEM) 28
3.3.2 穿透式電子顯微鏡(Transmission Electron Microscopy , TEM) 30
3.3.3 拉曼光譜儀(Raman Spectroscopy) 32
3.3.4 紫外光/可見光分光光譜儀(Ultraviolet–visible spectroscopy, UV/Vis ) 34
3.3.5霍爾效應量測儀 35
第四章結果與討論 38
4.1 石墨烯之拉曼光譜特性分析 38
4.1.1 改變氫氣流量成長石墨烯之拉曼光譜特性分析 40
4.1.2 不同甲烷流量成長石墨烯之拉曼光譜特性分析 44
4.1.3 反應區段改變氫氣流量成長石墨烯之探討 48
4.2成長寡層石墨烯之探討 49
4.3 以二氧化矽為基板成長石墨烯拉曼光譜特性分析 54
4.4 掃描式電子顯微鏡(SEM)形貌分析 56
4.5 Hall Effect量測 59
4.6 石墨烯穿透率分析 60
第五章結論 61
參考文獻 62

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