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研究生: 羅詩涵
Lo, Shih-Han
論文名稱: 寡層石墨烯剝離之環保製程技術開發
Development of an environmental process for exfoliating few-layer graphene
指導教授: 楊啟榮
Yang, Chii-Rong
吳俊緯
Wu, Jim-Wei
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: 94
中文關鍵詞: 寡層石墨烯熱震超音波震盪
英文關鍵詞: few-layer graphene, thermal-shock, sonication
DOI URL: https://doi.org/10.6345/NTNU202204160
論文種類: 學術論文
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  • 本研究提出一新穎環保之方法,利用剝離原始石墨即可獲得石墨烯,其中剝離方法包含熱震剝離與超音波震盪剝離兩種方法:熱震剝離方法具備快速升溫降溫的特性,適合應用於增加石墨層與層之間間距的效果;接下來藉由超音波震盪方法,再次增加石墨層與層之間距,並脫離凡德瓦力鍵,即獲得石墨烯。為與實驗結果進行比較,首先分別以拉曼光譜儀、場發射掃描式電子顯微鏡以及場發射穿透式電子顯微鏡檢測原始石墨之特性,其ID/IG比值為0.1845,層數則為100層以上。熱震剝離方法後,即可測得層數已降為20層以下,ID/IG比值為0.1926,證實熱震剝離方法並沒有造成石墨之結構損傷。再進行超音波震盪方法後,以離心篩選溶液,分別檢測8500 rpm樣品、3000 rpm樣品以及沉澱物樣品,ID/IG比值分別為0.2605、0.1753與0.3936,推測可能為進行超音波震盪方法時,使用含界面活性劑去離子水溶液,以避免機械剝離後所得之具疏水性石墨烯再次聚集,然而未完全清除界面活性劑,使ID/IG比值稍微提升。而由原子力顯微鏡檢測,三種樣品皆可得7層以下之寡層石墨烯,證實剝離方法確實具有將原始石墨剝離,並獲得寡層石墨烯之成效。

    In this study, we present a novel and environment method that can exfoliate the nature graphite into few-layer graphene. The exfoliation method includes both thermal-shock exfoliation method and sonication exfoliation method. The thermal-shock exfoliation method possesses the exceptional property that can heating and cooling rapidly, and it is good at raising the layers-spacing of nature graphite. The sonication exfoliation method raises the layers-spacing again, and disengages the van der Waals force between layer and layer, then we can obtain graphene. To compare with experimental results, first, we measure the property of nature graphite with Raman spectrometer, Field emission scanning electron microscope and Field emission transmission electron microscope, and obtain the value of ID/IG is 0.2605, the layers are above 100. After the thermal-shock exfoliation method, the layers of graphite are reducing under 20 layers, and the value of ID/IG is 0.1926. The results corroborate that the thermal-shock exfoliation method would not impair the structure of graphite. After the sonication exfoliation method, we discrete the sample by centrifugation and have 8500 rpm sample, 3000 rpm sample and residual sample. The value of ID/IG is 0.2605, 0.1753 and 0.3936, respectively. It is possible that we use the surfactant liquid to avoid the graphene which has hydrophobic property aggregate together again, but the surfactant liquid doesn’t eliminate clearly and causes the value of ID/IG increases slightly. The sample is measured with atomic force microscope, and the layers of all of them are under 7 years. It confirm that the exfoliation methods can exfoliate the nature graphite and attain the few-layer grapheme.

    摘要 I Abstract II 總目錄 III 表目錄 V 圖目錄 VI 第一章 緒論 1 1.1 前言 1 1.2 石墨烯常見製備方法 5 1.2.1 微機械剝離法 5 1.2.2 碳化矽表面磊晶法 7 1.2.3 化學氣相沉積法 9 1.2.4 氧化石墨剝離法 11 1.2.5 液相化學剝離法 15 1.3 研究動機與目的 17 1.5 論文架構 18 第二章 文獻回顧與理論探討 19 2.1 石墨烯製備技術 19 2.2 氧化石墨剝離法 22 2.2.1 快速加熱剝離法 24 2.2.2 超音波震盪剝離法 28 2.3 液相化學剝離法 34 第三章 實驗設計與規劃 42 3.1 研究設計 43 3.2 實驗細部規劃 46 3.3 製程與檢測設備 52 第四章 實驗結果與討論 58 4.1 石墨插層處理之參數最佳化 58 4.1.1 MA溶液參數最佳化 58 4.1.2 石墨濕潤性處理 59 4.1.3 石墨插層處理 60 4.1.4 去除石墨層間殘留氣體 64 4.2 熱震剝離處理 68 4.3 超音波剝離震盪熱處理 72 4.3.1 酸鹼中和去除殘留物 72 4.3.2 超音波震盪剝離處理 76 第五章 結論與未來展望 89 5.1 結論 89 5.2 未來展望 89 參考文獻 91

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