臺灣博碩士論文加值系統

在本論文中，我們利用鎳作為金屬觸媒以金屬附生法成長出多孔性石墨烯，另外亦以氣相沉積法成長之單層石墨烯作為氣體感測材料，進行氨氣以及數種有機氣體於ppm濃度等級之氣體感測。為了能夠有效達到氣體感測選擇性，我們更將多孔性石墨烯改質為氮摻雜之多孔性石墨烯以及多孔性石墨烯/多壁奈米碳管複合材料。在多孔性石墨烯的合成中，我們發現多孔性石墨烯的孔洞大小和成長時間有關係，成長時間少於10分鐘，其孔洞大小小於100奈米；而成長時間長於10分鐘，則可獲得1微米之孔洞結構。另外，所合成出的多孔性石墨烯薄膜屬於兩層至五層的多層石墨烯。而多孔性石墨烯改質的部分，我們成功地利用多孔性石墨烯缺陷邊緣誘發成長出多壁奈米碳管，其無須金屬觸媒進行催化反應，此外，透過30分鐘的氨氣熱處理，我們易成功的合成出氮摻雜多孔性石墨烯薄膜。最後，我們將上述不同石墨烯材料作為氣體感測元件進行無機以及有機氣體分子感測，發現單層石墨烯元件表現出最佳的氣體響應，其次為具有大孔洞之多層石墨烯元件，最後則為小孔洞之多層石墨烯元件。另外，有機性的氣體氣體響應比無機性的氣體響應來的高。另一方面，多壁奈米碳管/多孔性石墨烯複合材料之乙醇和異丙醇氣體響應較未改質石墨烯薄膜高，這是由於多壁奈米碳管/多孔性石墨烯複合材有更多的懸浮鍵結，而這些懸浮鍵結屬於更具反應力的吸附位置，因此能夠反應出更高的氣體響應；然而在丙酮氣體的量測，多壁奈米碳管/多孔性石墨烯複合材其氣體響應卻不增反降，這是由於丙酮分子感測機制和前兩者大不相同。氮摻雜石墨烯薄膜元件部分其氣體感測響應皆下降，這是因為氮摻雜量尚未達到將石墨烯轉換成n-type的量，反而使得石墨烯薄膜內部載子濃度下降。最後，我們提出不同於以往氣體選擇性的判斷，利用比較不同孔洞結構之石墨烯薄膜的氣體響應來達到氣體選擇性的偵測，因此我們相信其未來在電子鼻子(electronic nose)應用大有潛力。

Porous graphene films with tunable pore sizes and porosity are first demonstrated to be synthesized by solid state reactions with Ni catalytic thin films. These films together with single layer graphene (SLG) fabricated by chemical vapor deposition are compared in sensing behavior for NH3 and various organic vapors in ppm levels. All the gas sensing measurements involving adsorption/desorption behaviors of gases are carried out based on the change in electrical conductivity with different exposure times in different concentrations at room temperature. Raman spectroscopy, used to monitor the quality of the pristine graphene films, reveals the porous graphene to be mostly bilayer to five layer graphene. In general, the pore size of porous graphene decreases as decreasing the reaction time. Specifically, if the reaction time is less than 3 minutes, the distribution of pore size falls mainly in 10~100 nm, which increases to 1.2~1.6 um if the time prolongs to 10 minutes. For different vapor tested, the sensitivity of all types of graphene follows different order. Nevertheless, the sensitivity of the porous graphene with lager holes is higher than that with small pores for all types of gases, and the sensitivity of organic vapors is higher than inorganic vapors. Finally, we can compare all kinds of sensing devices to achieve the gas selectivity.

目錄

中文摘要 Ⅰ
英文延伸摘要 Ⅱ
致謝 Ⅶ
目錄 Ⅷ
表目錄 Ⅹ
圖目錄 ⅩⅠ
第一章 緒論 1
1-1 石墨烯的發展歷史 1
1-2 石墨烯的介紹 1
1-3 研究動機 4
第二章 文獻回顧 5
2-1 多孔性石墨烯合成方式 5
2-1-1 有機交聯鍵結 5
2-1-2 電漿/電子束/光子束蝕刻 7
2-1-3 模板附生 11
2-1-4 化學溶液蝕刻 12
2-2 氣體感測概論 17
2-2-1 金屬氧化物半導體材料應用於氣體感測 18
2-2-2 高分子應用於氣體感測 20
2-2-3 碳材料應用於氣體感測 22
2-3 石墨烯應用於氣體感測 26
2-3-1 石墨烯氣體感測機制 27
2-3-2 石墨烯應用於氣體感測 28
2-3-3 具缺陷石墨烯和官能基改質石墨烯應用於氣體感測 33
2-3-4 石墨烯複合材應用於氣體感測 38
2-3-5 發展瓶頸 40
第三章 實驗設備與步驟
3-1 實驗設備 43
3-1-1 精密離子蝕刻鍍膜系統 (Precision Etching Coating System, PECS) 43
3-1-2 真空退火爐系統 43
3-1-3 化學氣相沉積系統(Chemical Vapor Deposition, CVD) 44
3-1-4 氣體感測系統 45
3-1-5 微拉曼光譜儀(Micro-Raman) 46
3-1-6 高解析掃描式電子顯微鏡(High Resolution Scanning Electron Microscope, HR-SEM) 47
3-1-7 穿透式電子顯微鏡 (Transmission Electron Microscopy，TEM) 48
3-1-8 電性量測機台 48
3-2 實驗步驟 49
3-2-1 試片製備 49
3-2-2 熱退火處理 50
3-2-3石墨烯轉移 52
3-2-4 氮摻雜改質 53
3-2-5 成長奈米碳管改質 53
3-2-6 氣體感測 54
第四章 實驗結果與討論 55
4-1熱退火成長多孔性石墨烯 55
4-1-1成長多孔性石墨烯 55
4-1-2不同鎳金屬厚度及熱退火時間參數比較 57
4-1-3 多孔性石墨烯成長機制探討 69
4-2 多孔性石墨烯改質處理 72
4-2-1氮摻雜處理 72
4-2-2 奈米碳管成長處理 75
4-2-3 奈米碳管成長機制探討 79
4-3 氣體感測量測 81
4-3-1 未改質多孔性石墨烯氣體感測 81
4-3-2 未改質之多孔性石墨烯氣體感測機制討論 93
4-3-3 奈米碳管/多孔性石墨烯複合材氣體感測 96
4-3-4 氮摻雜處理多孔性石墨烯氣體感測 99
第五章 結論 100
第六章 參考文獻 101

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