臺灣博碩士論文加值系統

本研究所製備之Nafion包覆單壁奈米碳管修飾氧化亞銅之氧化鋅奈米柱/石墨烯複合材料於ITO玻璃上，成功應用於非酵素型葡萄糖感測器中。實驗主要將分為四個部分：第一部份為在氧化鋅奈米柱成長上採用不同厚度之晶種層，透過掃描式電子顯微鏡(Scanning Electron Microscope, SEM)觀測找出最佳參數；第二部分為利用電化學沉積氧化亞銅於氧化鋅奈米柱上，透過電化學量測找出最佳之電鍍時間；第三部分為添加Nafion所包覆之單壁奈米碳管(SWCNT)以增強對葡萄糖分子之捕捉能力；第四部份則是在氧化鋅奈米柱下先行製備一層石墨烯，並透過電化學量測來觀察石墨烯的加入是否會影響整體感測器的表現。
在0.1 M濃度之NaOH中以葡萄糖濃度50 mg/dL、100 mg/dL、150 mg/dL、200 mg/dL進行電化學循環伏安量測並將電壓在+0.8 V時之電流做紀錄，在氧化亞銅/氧化鋅奈米柱複合材料上對葡萄糖濃度與電流進行線性擬合，並測得其靈敏度(Sensitivity)為0.6207 μA mg-1 dL cm-2(約11.17 μA mM-1 cm-2)、R2值(擬合優越度)為0.9766。利用單壁奈米碳管與Nafion分散劑的作用下，增加感測器之表面積，並透過Nafion包覆之單壁奈米碳管增加對葡萄糖分子的捕捉能力，測得其靈敏度提升至16.1 μA mg-1 dL cm-2(約289.8 μA mM-1 cm-2)，且R2值(擬合優越度)高達0.992。
透過計時安培法(chronoamperometry)可得到當加入石墨烯在最底下時能使感測器得到兩個線性區間，分別是0-5.556 mM、靈敏度466.1 μA mM-1 cm-2與5.556-11.111 mM、靈敏度203.1 μA mM-1 cm-2，其R2值分別為0.9917與0.9777。

The non-enzymatic glucose sensor was successfully prepared in this research which the single-wall carbon nanotubes (SWCNTs) were wrapped with Nafion to enhance the sensitivity of sensor based on the copper(I) oxide (Cu2O) surface modification of zinc oxide nanorod (ZnO NR)/Graphene composites on ITO glass. The experimental procedure of this research has four steps: First, the different sputtering time was used to deposit the ZnO seed layer, and then will be synthesis ZnO NR by hydrothermal. The morphology of ZnO NR was checked by scanning electron microscope (SEM). Secondly, the optimal cupreous time of Cu2O on the ZnO NR would be verified by electrochemistry with the different concentration of glucose. Thirdly, the SWCNTs wrapped with Nafion was dropped to Cu2O /ZnO NR to increase the catching ability of the glucose and checked by electrochemistry. Lastly, graphene would be prepared on the ITO glass and then fabricated the Cu2O surface modification of ZnO NR/Graphene composites.
In the electrochemistry measurement, 0.1M NaOH was used as the electrolyte, and there were four concentrations of glucose: 0, 100, 150 and 200 mg dL-1. The electrochemical characteristics of the sensors were investigated by cyclic voltammetry (CV). The results showed the modified electrodes of Cu2O/ZnO NR had a linear response to glucose concentration and the maximum concentration could reach to 200 mg/dL with the sensitivity of 0.6207 μA mg-1 dL cm-2(about 11.17 μA mM-1 cm-2). Because the SWCNTs wrapped with Nafion could enhance the capturing ability of glucose checked by the CVs curve of electrochemistry. Since, the modified electrodes of SWCNT/Cu2O/ZnO NR has the optimal linear range from 0 to 200 mg/dL and good sensitivity of 16.1 μA mg-1 dL cm-2(289.8 μA mM-1 cm-2). Anyway, the SWCNTs wrapped with Nafion could increase the sensitivity of glucose sensor.
The chronoamperometry (CA) is a precision real time response of the glucose sensor. So the graphene was fabricated on the ITO glass to adhesive on the SWCNTs/Cu2O/ZnO NR/Graphene composites as the glucose sensor, then the sensor would be tested by the CA method with the increasing the glucose concentration. The calibration curve of glucose sensor has two linear ranges: 0-5.556 and 5.556-11.111 mM and have the sensitivity of 466.1 and 203.1 μA mM-1 cm-2, respectively. The addition of graphene could increase the sensitivity at low concentration and reduce the response time (< 2 s) for the SWCNTs/Cu2O/ZnO NR glucose sensor.

摘要 i
ABSTRACT ii
誌謝 iii
目錄 iv
表目錄 vii
圖目錄 viii
第一章　緒論 1
1-1 前言 1
1-2 研究動機 5
1-3 研究方法 7
第二章　文獻回顧 8
2-1 感測器簡介 8
2-2 感測器種類 10
2-2-1 物理感測器 10
2-2-2 化學感測器 10
2-2-3 生物感測器 10
2-3 生物感測器 12
2-4 奈米碳管 18
2-4-1 奈米碳管結構 18
2-4-2 奈米碳管合成方式 18
2-5 石墨烯 22
2-5-1 石墨烯介紹 22
2-5-2 石墨烯合成方式 22
2-6 氧化鋅奈米柱 31
2-6-1 氧化鋅特性 31
2-6-2 氧化鋅合成方式[50-53] 32
2-7 氧化亞銅 37
2-8 葡萄糖生物感測器 39
第三章　實驗方法與步驟 40
3-1 實驗流程 40
3-2 實驗藥品及耗材 42
3-3 儀器設備介紹 43
3-3-1 冷場發射掃描式電子顯微鏡(Cold Field Emission Scanning Electron Microscope, FE-SEM) 43
3-3-2 X光繞射儀(X-ray diffraction, XRD) 44
3-3-3 拉曼光譜儀(Raman spectrometer) 45
3-3-4 光柵光譜儀(UV/Visible Spectrophotometer) 47
3-3-5 電化學分析儀(Electric chemistry analyzer) 49
3-4 實驗步驟及方法 51
3-4-1 基板清洗 51
3-4-2 利用化學氣相沉積法成長石墨烯 52
3-4-3 製備氧化鋅晶種層 54
3-4-4 熱退火 56
3-4-5 水熱法合成氧化鋅奈米柱 57
3-4-6 非酵素型葡萄糖感測器製作 58
3-4-7 奈米碳管溶液配置 61
第四章　結果與討論 63
4-1 熱化學氣相法成長石墨烯 63
4-2 氧化鋅晶種層與氧化鋅奈米柱之製備 65
4-1-1 光柵光譜儀分析氧化鋅晶種層與氧化鋅奈米柱 65
4-1-2 Raman 光譜分析 68
4-1-3 氧化鋅奈米柱之SEM表面形貌 70
4-1-4 X光繞射儀(X-ray diffraction, XRD) 74
4-3 氧化亞銅(Cu2O)/氧化鋅奈米柱(ZnO NR)複合材料 77
4-3-1 製備氧化亞銅於ITO玻璃 77
4-3-2 製備氧化亞銅於氧化鋅奈米柱 79
4-3-3 SEM分析氧化亞銅/氧化鋅奈米柱其表面形貌 81
4-3-4 Raman 光譜分析 84
4-3-5 X光繞射儀分析 85
4-3-6 電化學儀量測 86
4-4 奈米碳管/氧化亞銅/氧化鋅奈米柱複合材料應用於非酵素型葡萄糖感測器 91
4-4-1 Raman光譜檢測奈米碳管/Nafion固定劑溶液 91
4-4-2 電化學儀量測 92
4-5 奈米碳管/氧化亞銅/氧化鋅奈米柱/石墨烯複合材料應用於非酵素型葡萄糖感測器 97
4-6 非酵素型葡萄糖感測器之比較 103
第五章　結論 105
參考文獻 107

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