低溫還原氧化石墨烯薄膜

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姓名

黃怡雯(Yi-Wen Huang) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

低溫還原氧化石墨烯薄膜
(Low-Temperature Reduction of Thin Graphene Oxide Film)

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摘要(中)

本研究是將市售的石墨片以電解剝落法製備微奈米級的石墨/石墨烯，再藉由電泳沉積法製備石墨烯薄膜於不鏽鋼片上。電泳沉積藉由電解剝落法所得到的氧化石墨/石墨烯奈米粒子因表面所帶的負電而穩定懸浮於溶液中，在經由施加一電場後使之沉積在正電極而形成薄膜。實驗中經由電解剝落法中的電解液選擇、粒子粒徑大小的過濾及電壓大小的調控得到一細緻且平整之石墨烯薄膜，其厚度約為1μm。另外本實驗也以蒸發沉積法將石墨烯粒子沉積在非導電基材上，並且可藉此方式形成一可撓式石墨烯薄膜。實驗中利用兩種方式還原薄膜，分別是真空還原及酒精還原，前者將薄膜置於真空中加熱至100℃一小時，後者將薄膜置於220℃酒精蒸氣中使其還原；還原薄膜以接觸角量測儀分析，其接觸角由38°提升至83°，實驗中也以XPS、TGA、XRD、Raman儀器鑑定顯示所製備的石墨烯薄膜已達到部分還原的效果，並且由酒精還原之石墨烯薄膜還原效果最好。最後經由四點探針量測還原後薄膜電阻率可達9×10^(-4) Ω∙cm。

摘要(英)

The graphene oxide nanoparticles obtained from anodic graphite by electrochemical exfoliation, followed by electrophoretic deposition onto stainless steel or nickel substract. Another way to deposit graphene particles on non-conductive substract is used to produce graphene film, which named Evaporative Deposition(ED). By ED, graphene films can be deposit on polymer substracts like PEN and formed a flexible graphene film. The graphite film formed was reduced in two ways, vacuum treatment with heating up to 100℃ and ethanol treatment with heating up to 220℃. The wetting properties are determined by contact angle measurement. The advancing and receding contact angles of graphene oxide film are 38.4° and 15.5o, respectively. This result reveals the thin film is rather hydrophilic. After the reduction treatment, the advancing and receding contact angle increased to 83.1° and 50.5°, respectively, indicating that the surface of graphene oxide film becomes more hydrophobic. By the analysis of TGA, Raman, XRD and XPS, the results proved that both of the reduction treatment had attained a reduction effect. After the reduction, a graphene film was obtained and the resistivity of the film is 9×10^(-4) Ω∙cm.

關鍵字(中)

★ 石墨烯
★ 還原

關鍵字(英)

★ Graphene
★ Reduction

論文目次

摘要 i
Abstract ii
致謝 iii
圖目錄 vii
表目錄 x
第1章緒論 1
1-1 石墨 1
1-2 石墨烯 2
1-3 相關文獻回顧 3
1-4 研究動機與目的 7
第2章原理介紹 8
2-1 石墨烯之製備 8
2-2 電解剝落法 11
2-3 電解剝落法之原理 12
2-4 電泳沉積法 12
2-4-1 電泳沉積法之原理 13
2-5 咖啡漬圈環效應(Coffee Ring Effect) 14
第3章理論背景 16
3-1 潤濕現象 16
3-1-2 表面潤濕現象 17
3-2 潤濕現象的定義 18
3-2-1 楊式方程式(Young′s equation) 18
3-2-2 溫佐方程式( Wenzel′s equation ) 21
3-2-3 卡西方程式(Cassie′s equation) 23
3-3 接觸角遲滯現象(Contact angle hysteresis) 24
3-3-2 接觸角遲滯的定義 26
3-3-3 遲滯現象的原理 27
3-4 動態接觸角(Dynamic contact angle) 29
3-5 潤濕現象的量測方式 29
3-5-1 微量針頭法( Needle-Syringe ) 29
3-5-2 蒸發法(Evaporation method) 30
3-5-3 Wilhelmy 平板法( Plate Method ) 32
3-5-4 傾斜法 ( Inclined plate ) 32
第4章實驗介紹 34
4-1 實驗藥品及材料 34
4-2 實驗儀器 35
4-2-1 影像式接觸角測量儀 37
4-2-2 分光光譜儀 (UV) 37
4-2-3 動態光散射 (Dynamic light scattering) 39
4-2-4 熱重分析儀 (TGA) 39
4-2-5 光電子能譜儀 ( XPS, mapping ,depth profile ) 39
4-2-6 X光粉末繞射儀 (X-ray Diffractometer，簡稱XRD) 40
4-2-7 拉曼 (Raman) 40
4-2-8 三維量測儀 (Alpha-step) 41
4-2-9 四點探針 41
4-3 實驗方法 42
4-3-1 材料實驗前處理 42
4-3-2 電解剝落之實驗步驟 42
4-3-3 電泳沉積之實驗步驟 42
4-3-4 蒸發沉積之實驗步驟 43
4-3-5 石墨烯薄膜還原之實驗步驟 43
第5章結果與討論 44
5-1 不同酸鹼性之電解液對電泳沉積之影響 44
5-2 不同粒徑大小及電壓對電泳沉積之影響 48
5-2-1 粒徑大小對電泳沉積之影響 48
5-2-2 電壓大小對電泳沉積之影響 48
5-3 石墨烯薄膜之還原 51
5-3-1 低溫抽真空以還原石墨烯薄膜 51
5-3-2 低溫酒精蒸氣還原石墨烯薄膜 52
5-4 石墨烯薄膜還原之驗證 57
5-5 蒸發沉積法 (Eavporative Deposition) 65
5-6 薄膜性質之比較 70
第6章結論 72
第7章參考資料 74

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指導教授

曹恆光(Heng-Kwong Tsao)

審核日期

2015-6-11

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