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研究生： 陳昱廷
Chen, Yu-Ting
論文名稱： 氧化石墨烯的電能還原技術開發
Reduced techniques of graphene oxide developed using electric energy
指導教授： 楊啟榮
Yang, Chi-Rong
曾釋鋒
Tseng, Shih-Feng
學位類別： 碩士
Master
系所名稱： 機電工程學系
Department of Mechatronic Engineering
論文出版年： 2016
畢業學年度： 104
語文別： 中文
論文頁數： 118
中文關鍵詞： 石墨烯 、氧化石墨烯 、電漿還原技術
英文關鍵詞： Graphene, Graphene oxide, Plasma reduction technology
DOI URL： https://doi.org/10.6345/NTNU202204880
論文種類： 學術論文
相關次數： 點閱：158  下載：4 
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    • 本研究提出一個新穎的方法，使用電能來還原氧化石墨烯，其中電能包含了電弧放電與常壓電漿兩種方法，兩種方法均具備了升溫快速、高能量等特性，適合應用於還原氧化石墨烯。首先，本研究以Improved Hummers method製備氧化石墨烯，所製備出的氧化石墨烯其ID/IG之比值為0.77，C/O為0.232，電阻值為280 MΩ，並將自製之氧化石墨烯，分別製備出粉末、分散液及薄膜形式，再以電弧與電漿分別進行實驗，使用拉曼、電性、比表面積及XPS評估其特性，最後與UV雷射所還原之氧化石墨烯納入比較。本研究在進行電弧放電的實驗中，發現有儀器性能上的限制，導致還原成效不彰，因此將實驗重心移至常壓電漿還原實驗。透過常壓電漿系統，成功還原氧化石墨烯，氧化石墨烯薄膜在處理時間為2小時的情況下，其電阻值由280 MΩ下降至1657 Ω，電性明顯的提升，I2D/IG之比值由0增加至0.05，此外，將石英玻璃作為遮蔽物使用於還原實驗中，因薄膜的完整性大幅提升，因此電阻值在處理時間為2小時的情況下，由1657 Ω下降至141 Ω，I2D/IG之比值提升至0.3，還原的效果十分良好。實驗結果顯示，電漿還原後觀察氧化石墨烯其電性的提升，證明確實具有還原之成效，結合石英玻璃作為遮蔽物進行電漿處理，更能大幅改善其電性。

    In this study, we present a novel method that uses electric energy to turn graphene oxide into reduced grpahene oxide. The electric energy which contains the arc discharge and atmospheric plasma two methods, both methods have an advantage of rapid heating, high energy and other characteristics. It is suitable for reduce graphene oxide. First, we used the present study Improved Hummers method for preparing graphene oxide. the graphene oxide prepared ID ratio IG is 0.77, carbon to oxygen ratio is 0.232, and the resistance is 280 MΩ. Moreover, the homemade of graphene oxide was prepared for powders, dispersions and film form, respectively. Then the arc discharge and plasma were conducted to experiments. Finally, it will used Raman, electrical resistance, specific surface area and XPS analysis to estimate its characteristics. In the end, it will be compared with reduction effect which is using UV laser to reduce. This study has faced some critical problems during arc discharge experiments. Due to the performance restrictions of instrument can’t be improved. So the resulting of reduction isn’t very effective. Hence, the experiment will focus to the plasma experiments. Through the atmospheric plasma system, it is successfully restored graphene oxide, graphene oxide film under two hours processes time in the case, the resistance value decreased from 280 MΩ to 1657 Ω. The electrically improved significantly, the I2D ratio IG increase from 0 to 0.05. Besides, quartz glass as shelter has used in the reducing experiment, because the integrity of the film is significantly improved. The resistance value decreased from 1657 Ω to 141 Ω. I2D ratio IG increased to 0.3, the reduction of the effect is very good. Experimental results show that electrical properties of reduced graphene oxide is better than GO after plasma treatment, has indeed proved it contains reduction effect. If we combined quartz glass as a shelter with plasma experiment, it will more significantly improve its electrical properties.

    摘要 ........................................................................................................................ I Abstract ............................................................................................................... II 總目錄 ................................................................................................................ III 表目錄 ................................................................................................................ VI 圖目錄 ............................................................................................................... VIII 第一章 緒論 ....................................................................................................... 1 1.1 前言............................................................................................................. 1 1.2 石墨烯製備簡介 ........................................................................................ 3 1.2.1 微機械剝離法 .................................................................................. 3 1.2.2 化學汽相沉積法 .............................................................................. 4 1.2.3 碳化矽熱裂解磊晶法 ...................................................................... 7 1.2.4 化學剝離法 .................................................................................... 10 1.2.5 電化學剝離法 ................................................................................ 12 1.2.6 氧化石墨化學剝離法 .................................................................... 15 1.3 石墨烯未來發展 ...................................................................................... 17 1.4 研究動機與目的 ...................................................................................... 18 1.5 論文架構 .................................................................................................. 19 第二章 文獻回顧與理論探討 ..................................................................... 20 2.1 氧化石墨烯的還原方法回顧 ................................................................... 20 2.1.1 化學藥劑還原法 ............................................................................ 21 2.1.2 光觸媒還原法 ................................................................................ 25 2.1.3 電化學還原法 ................................................................................ 26 2.1.4 高溫熱退火還原法 ........................................................................ 28 2.1.5 微波照射還原法 ............................................................................ 30 2.1.6 雷射照射還原法 ............................................................................ 32 2.1.7 複合還原法 .................................................................................... 37 2.2 電弧放電原理 ........................................................................................... 40 2.3 電弧放電剝離石墨烯 ............................................................................... 44 第三章 實驗設計與規劃 ................................................................................ 46 3.1 實驗設計 .................................................................................................. 46 3.2 實驗規劃 .................................................................................................. 53 3.3 實驗與檢測設備 ...................................................................................... 58 第四章 實驗結果與討論 ................................................................................ 65 4.1氧化石墨之製作結果 ............................................................................... 65 4.1.1石墨預氧化處理 ............................................................................. 65 4.1.2 深層氧化處理 ................................................................................ 67 4.1.3 後處理 ............................................................................................ 69 4.1.4 氧化石墨烯分析 ............................................................................ 73 4.2雷射還原氧化石墨烯 ............................................................................... 77 4.2.1雷射還原樣品選擇 ......................................................................... 77 4.2.2雷射功率對於還原之影響 ............................................................. 82 4.2.3掃描次數對於還原之影響 ............................................................. 88 4.3電能還原氧化石墨烯 ............................................................................... 93 4.3.1電弧還原實驗結果 ......................................................................... 93 4.3.2電漿還原實驗結果 ....................................................................... 101 4.3.2.1 製程時間對於還原之影響 ............................................ 101 4.3.2.2 遮蔽物對於還原之影響 ................................................ 105 第五章 結論與未來展望 .............................................................................. 112 5.1結論 .................................................................................................. 112 5.2未來展望 .......................................................................................... 112 參考文獻 .......................................................................................................... 114

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