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研究生： 許馨予
Hsin-Yu Hsu
論文名稱： 紫外光臭氧處理和ITO奈米顆粒改質石墨烯 應用於光及氨氣感測器
Graphene Modified by UV/ozone Treatment and ITO Nanoparticles as Photodetector and Ammonia Sensor
指導教授： 周賢鎧
Shyan-Kay Jou
口試委員: 黃柏仁
Bohr-Ran Huang
胡毅
Hu Yi
學位類別： 碩士
Master
系所名稱： 工程學院 - 材料科學與工程系
Department of Materials Science and Engineering
論文出版年： 2021
畢業學年度： 109
語文別： 中文
論文頁數： 202
中文關鍵詞： 石墨烯 、紫外光臭氧處理 、氧化銦錫 、蕭特基元件 、氨氣感測器 、光感測器
外文關鍵詞： UV/ozone Treatment, ITO, Ammonia Sensor, Photodetector
相關次數： 點閱：391  下載：0 
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    • 本研究透過化學氣相沉積法生成雙層石墨烯，並利用兩種改質方式修飾石墨烯，一種為紫外光臭氧處理，可以提高石墨烯表面含氧官能基，增加氨氣吸附能力及光電子轉移效果，另一種為濺鍍ITO奈米顆粒於表面，適當分布的奈米顆粒不只可以提高氣體分子吸附，由顆粒表面解吸的氧離子，亦可增加光照時的光電流。兩種改質方法以拉曼進行分析，可以發現ID/IG會變大，而I2D/IG變小，皆會對石墨烯造成缺陷。除此之外，會透過UV-visible、AFM、XPS進行改質石墨烯之分析，了解改質方法對石墨烯產生之其他影響。
    本實驗的氨氣感測結果，在UVO處理改質方面，經過15分鐘處理時間之元件於50 ppm的氨氣濃度下有14.8 %的響應度，高於原石墨烯的2.6 %，而響應時間為58.3 s，回復時間為106.2 s，皆快於原石墨烯所花費的時間，因為增加的含氧基團數量能夠有效吸附氨氣氣體分子，提高其響應度。在ITO顆粒沉積方面，以30 W濺鍍30 s的樣品，於50 ppm的氨氣濃度下有8 %的響應度，高於原石墨烯，其響應時間為40.0 s，回復時間為124.7 s，亦較原石墨烯所花費的時間短，這是因為ITO奈米顆粒存在，不只可以提高氨氣吸附能力，P-type的ITO與N-type石墨烯接觸，可以產生p-n界面，加快電子傳輸效果。
    實驗進一步量測光感測性能，發現元件具有 self power 特性，且開關比在UVO處理之元件可以高達106，濺鍍ITO的元件可以達到105。另外，比較其響應度及外部量子效應得知，改質之石墨烯皆有較大的數值。UVO處理後更為寬廣的能隙，可以增加吸收光子的能力；在光照射下ITO顆粒內電子會被激發而躍遷，產生自由電子生成強電流，增加石墨烯對光的響應。基於上述結果，UVO處理及濺鍍ITO 奈米顆粒皆可有效提升石墨烯作為光與氨氣感測器之響應。

    In this study, bi-layer graphene was grown by chemical vapor deposition, and two modification methods were used to modify graphene. One is UV/ozone treatment. This way can increase the active oxygen functional groups on the graphene surface, which can efficiently act as adsorption sites for detected gas molecules. The other one is depositing ITO nanoparticles on the surface. It can not only increase the adsorption of gas molecules, but the oxygen ions desorbed from the surface of the particles can also increase the current during light exposure. We can find that ID/IG become larger and I2D/IG become smaller from Raman spectroscopy by modifying. As to show that more defects have been created in graphene. In addition, UV-visible, AFM, and XPS were conducted to understand other effects of modification methods on graphene.
    The result of ammonia gas sensing in this experiment, the response is about 14.8 % for UVO treated 15 min Schottky device, It is higher than PG of about 2.6 % to 50 ppm NH3. UVO 15’s response time is 58.3 s and the recovery time is 106.2s, which is faster than the pure graphene one. In terms of ITO nanoparticles deposition, the 30W-30s-ITO based ammonia sensor at 50 ppm exhibit response of 8%. The response time is 40.0 s and the recovery time is 124.7 s, which are also better one. Because the p-n interface between the n-type ITO and the p-type graphene produces a stepwise energy barrier, electrons can pass through the stepped energy barrier more quickly.
    For the photodetector, the device show the self-powered characteristic. The ON/OFF ratio of UVO-treated’s responsivity can achieve up to 106. The ON/OFF ratio of ITO deposition’s responsivity can achieve up to 105. In addition, graphene modified by UV/Ozone treatment and ITO nanoparticles have a larger value on responsivity and external quantum efficiency. The wider energy gap after UVO treatment can increase the ability to absorb photons. The ITO particles’s electrons become excited state under the light. It generates strong current and increas the response of graphene. Based on the above results, we know that both UVO treatment and ITO nanopartical can effectively improve the response of graphene as a photodetector and ammonia sensor.

    摘要 i Abstract ii 致謝 iv 目錄 vi 表目錄 xi 圖目錄 xiv 第一章 前言 1 1.1. 生活隨處可見之光感測裝置 1 1.2. 大氣中的空氣汙染與毒性氣體 2 1.3. 研究動機 2 第二章 文獻回顧 3 2.1 晶體結構與特性 3 2.1.1. 石墨烯晶體結構與特性 3 2.1.2. 氧化石墨烯的晶體結構與特性 4 2.2 製備方法 5 2.2.1. 石墨烯的製備方法 5 2.2.1.1 磊晶成長法（Epitaxial growth） 6 2.2.1.2 氧化石墨烯還原法（Graphene oxide reduction） 6 2.2.1.3 機械剝離法（mechanical exfoliation） 6 2.2.1.4 化學氣相沉積法（Chemical vapor deposition, CVD） 7 2.2.2. 石墨烯之氧化改質 8 2.2.2.1 焊馬方法(Hummers’method) 9 2.2.2.2 氧電漿處理(oxygen plasma treatment) 9 2.2.2.3 紫外光臭氧處理(UV/Ozone treatment) 10 2.3 石墨烯及氧化石墨烯的拉曼光譜分析 12 2.3.1. 石墨烯拉曼光譜 12 2.3.2. 氧化石墨烯拉曼光譜圖 13 2.4 石墨烯之蕭特基元件探討 15 2.5 結合ITO奈米顆粒與石墨烯 17 2.6 石墨烯製備之氣體感測器 18 2.6.1. 純石墨烯氣體感測器之特性 18 2.6.2. 改質之氧化石墨烯的氣體感測器特性 21 2.6.3. 氧化金屬奈米顆粒/石墨烯之氣體感測器特性 24 2.7 石墨烯製備之光感測器 30 2.7.1 純石墨烯光感測器之特性 31 2.7.2 改質之氧化石墨烯的光感測器特性 32 2.7.3 氧化金屬奈米顆粒/石墨烯之光感測器特性 33 第三章 實驗方法與實驗儀器 36 3.1. 實驗材料與藥品規格 36 3.2. 實驗設備與儀器 38 3.3. 實驗步驟 38 3.3.1. 基材清洗 38 3.3.2. 化學氣相沉積法生長石墨烯 39 3.3.3. 轉移石墨烯至特定基板 41 3.3.4. 製備蕭特基(Schottky)元件 42 3.3.5. 製備氧化石墨烯 44 3.3.6. 磁控式濺鍍ITO製程 44 3.4. 實驗裝置與分析儀器 45 3.4.1. 實驗裝置與分析儀器 45 3.4.2. 化學氣相沉積系統（Chemical Vapor Deposition system） 47 3.4.3. 磁控式濺鍍系統（Magnetron Sputtering） 47 3.4.4. 紫外光臭氧清洗機 (UV/Ozone cleaner) 47 3.4.5. 顯微拉曼光譜儀（Microscopes Raman Spectrometer） 48 3.4.6. 場發射掃描式電子顯微鏡（Field Emission Scanning Electron Microscope, FE-SEM） 49 3.4.7. X射線光電子能譜儀（X-ray Photoelectron Spectroscopy, XPS） 50 3.4.8. 原子力顯微鏡（Atomic force microscope, AFM） 51 3.4.9. 紫外光可見光光譜儀(Ultraviolet-visible spectrometer, UV-vis) 52 3.4.10. 光感測器量測系統(Photodetector system) 53 3.4.11. 氣體感測器量測系統（Gas Sensing System） 54 第四章 結果與討論 55 4.1. 紫外光臭氧處理石墨烯之結果分析 55 4.1.1. 拉曼光譜結果分析 55 4.1.2. XPS結果分析 57 4.1.3. 紫外可見光光譜圖分析 67 4.1.4. AFM結果分析 69 4.1.5. 蕭特基元件暗室電性分析 72 4.1.6. 氨氣感測分析 74 4.1.6.1 氧化石墨烯之靜態分析 74 4.1.6.2 氨氣感測效應與探討 78 4.1.7. 光感測分析 83 4.2. ITO處理之結果分析 93 4.2.1. 拉曼結果分析 93 4.2.2. XPS結果分析 94 4.2.3. 紫外可見光光譜圖分析 106 4.2.4. AFM結果分析 107 4.2.5. 蕭特基元件暗室電性分析 109 4.2.6. 氨氣感測分析 114 4.2.6.1 ITO/石墨烯之靜態分析 114 4.2.6.2 氨氣感測效應與探討 116 4.2.7. 光感測分析 119 第五章 結論 128 第六章 未來展望 132 參考文獻 133 附錄 140 附錄一、 蕭特基元件於乾燥空氣暗室之電性分析，PG 及經過 UVO 處理石墨烯之(a) I-V 曲線與(b) ln(J)-V 關係圖。 140 附錄二、 各組UVO處理元件暴露於不同氨氣濃度下的I-V曲線圖及在+3 V偏壓時的各濃度電流變化。 142 附錄三、 各組UVO處理元件暴露於不同氨氣濃度下的semilog I-V曲線圖及局部放大圖。 145 附錄四、 UVO處理元件於乾燥空氣環境對氨氣感測之分析。 148 附錄五、 PG及UVO處理後樣品之R值、EQE值趨勢圖。 156 附錄六、 經過UVO處理元件以強度0.3 mW/cm2 、501 nm 波長的LED照射下，利用示波器量測之V-t 圖。 157 附錄七、 PG及各組ITO元件之[C][O]原子比例。 160 附錄八、 各組ITO元件暴露於不同氨氣濃度下的I-V曲線圖及在+3 V偏壓時的各濃度電流變化。 161 附錄九、 各組ITO元件暴露於不同氨氣濃度下的semilog I-V曲線圖及局部放大圖。 163 附錄十、 各組ITO之元件於乾燥空氣環境對氨氣感測之分析。 165 附錄十一、 濺鍍ITO元件以強度0.3 mW/cm2 、501 nm 波長的LED照射下，利用示波器量測之V-t 圖。 171 附錄十二、 UVO 15 min於395、632、850 nm光源照射下進行動態氣體感測。 173 附錄十三、 ITO 30W-30s於395、632、850 nm光源照射下進行動態氣體感測。 177 附錄十四、 UVO處理的蕭特基元件之dV/dlnJ v.s J及H(J) v.s J圖。 181 附錄十五、 ITO處理的蕭特基元件之dV/dlnJ v.s J及H(J) v.s J圖。 183

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