臺灣博碩士論文加值系統

為了改善傳統轉置方法對石墨烯品質所帶來的影響，本研究目標於二氧化矽基板上濺鍍銅薄膜作為化學氣相沉積製程中的催化金屬，並將此鍍有銅膜的矽基板置於一具有狹縫的石英載具中，利用狹縫所提供的侷限空間進行免轉置石墨烯的成長。透過調控成長溫度、腔體壓力、退火時間、製程氣體比例、成長時間等合成參數，再以鎳片覆蓋銅膜做為吸收多餘碳源的儲存槽（carbon sink）合成出高品質的免轉置石墨烯。本研究於反應溫度1000 ℃與腔體壓力為90 torr的環境下，以厚度700 nm的銅膜作為催化基材，並置於具有0.55 mm凹槽深度的石英狹縫中，以鎳片覆蓋銅膜，成功的不需透過轉置步驟直接成長高品質的雙層石墨烯於矽基板上。
此外，免轉置石墨烯在蝕刻過程中發現因無支撐層保護溶液產生石墨烯薄膜破損問題導致後續無法正確評估合成參數對於石墨烯品質與層數的影響，因此也開發了微流道蝕刻系統以層流的方式進行蝕刻成功避免了石墨烯薄膜破損的問題。此外，在實驗過程中發現因使用石英管作為化學氣象沈積腔體，導致成長過程中有大量矽奈米球沉積在銅膜基板上進而汙染所合成的石墨烯薄膜，，為了解決矽球污染問題，稀釋的KOH溶液被使於微流道的系統中，於去除銅膜前，先對銅膜上沈積的矽奈米球進行清洗蝕刻，解決了石墨烯受矽球汙染的問題。

Conventional processes to transfer chemical vapor deposited graphene from catalytic metal surface to dielectric substrates are typically involved in introduction of defects and contaminations onto the as-grown graphene, resulting in deteriorated graphene quality. To solve this problem, it is inevitable to develop a practical transfer-free process to directly grow graphene on target substrates. In this study, we propose to synthesize graphene using a deposited Cu film on the silica substrate to enable transfer-free growth of graphene film via CVD method. The key of our strategy is to utilize a quartz slit as a confined space where the Cu/Si substrate is located and a Ni sheet as the slit cover on top of the Cu/Si substrate to locally control the carbon source supply. To prepare high-quality transfer-free graphene we systematically studied the effects of the following parameters, including growth temperature, chamber pressure, annealing time, reaction gas ratio, growth time, gap size of the quartz slit to optimize the synthesis process. Consequently, we successfully synthesized patterned transfer-free graphene at 1000 ℃ under a chamber pressure of 90 torr by covering the Ni sheet on a Cu metal film with a total thickness of 700 nm in a 0.55 mm quartz slit. According to the statistical analysis of Raman measurements recorded from the synthesized graphene films, we demonstrated that the produced transfer-free graphene composed of ~2 layered graphene films. In addition, we have developed a microchannel etching system to remove the deposited Cu film in a laminar flow to prevent breakage of graphene film during the etching process. Furthermore, dilute KOH solution was applied before the Cu etching process to remove the contamination of SiO2 nanospheres deposited on the Cu film, a problem frequently encountered in conventional CVD process using quartz tube as the reaction chamber, to further improve the quality of synthesized graphene.

摘要 I
Extended Abstract II
誌謝 XI
目錄 XII
圖目錄 XV
表目錄 XXI
第一章 緒論 1
第二章 文獻回顧 2
2.1 石墨烯簡介 2
2.1.1 基本性質 2
2.1.2 發展背景 4
2.2 石墨烯結構與特性 6
2.2.1 物理特性 6
2.2.2 晶格結構14-15 7
2.2.3 能帶結構 8
2.3 石墨烯製備方法 9
2.3.1 機械剝離法 9
2.3.2 碳化矽磊晶成長法 10
2.3.3 氧化石墨（烯）還原法 11
2.3.4 液相剝離法 13
2.3.5 電化學剝離法 14
2.3.6 化學氣相沉積法 15
2.4 化學氣相沉積製備石墨烯 17
2.4.1 化學氣相沉積種類 17
2.4.2 石墨烯成長於過渡金屬上 21
2.4.3 石墨烯成長於鎳基板上 22
2.4.4 石墨烯成長於銅基板上 23
2.5 石墨烯轉置方法 26
2.5.1 聚合物支撐層轉置法 26
2.5.2 熱解膠帶轉置法 34
2.5.3 無聚合物轉置法 37
2.6 免轉置石墨烯方法 41
2.7 石墨烯檢測方法 56
2.7.1 光學散射 56
2.7.2 拉曼光譜 58
2.8 研究動機與目標 64
第三章 實驗方法與材料 65
3.1 實驗流程設計 65
3.2 濺鍍銅薄膜於矽基板實驗步驟 66
3.2.1 光罩設計 66
3.2.2 光阻製程 67
3.2.3 濺鍍金屬基材 68
3.2.4 舉離光阻 68
3.3 化學氣相沉積製備石墨烯 69
3.3.1 銅鍍膜基板處理 69
3.3.2 化學氣相沉積系統架構 69
3.3.3 化學氣相沉積製程參數 70
3.4 免轉置石墨烯方法 71
3.5 檢測儀器 72
3.5.1 光學顯微鏡 （optical microscopy, OM） 72
3.5.2 拉曼顯微鏡 （Raman microscopy） 72
3.5.3 掃描式電子顯微鏡 （scanning electron microscopy, SEM） 73
3.5.4 原子力顯微鏡（atomic force microscopes, AFM） 73
第四章 結果與討論 74
4.1 銅膜厚度鑑定 77
4.2 腔體壓力控制 77
4.3 成長溫度影響 80
4.4 退火時間影響 82
4.5 甲烷流量對成長的影響 84
4.6 氫氣流量對成長影響 86
4.7 氬氣流量對成長影響 88
4.8 成長時間之影響 90
4.9 反應腔體總壓影響 92
4.10 銅膜厚度影響 94
4.11 狹縫載具限縮空間影響 97
4.12 鎳金屬催化劑對石墨烯成長影響 99
4.13 圖案化石墨烯的成長 106
4.14 微流道蝕刻改良 107
4.15 矽球汙染改善 110
第五章 總結與未來展望 112
第六章 參考文獻 113

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