臺灣博碩士論文加值系統

本次研究以無機金屬氧化物半導體材料作為主題，再以奈米結構方式增加感測葡萄糖面積，做為此次非酵素葡萄糖感測電極，並且改善酵素型電極的缺點，提升再電化學偵測葡萄糖的反應靈敏度與穩定性。
本研究分三階段，第一階段使用水熱法製備氧化鋅奈米柱用來比較量測不同濃度氫氧化鈉溶液下量測葡萄糖感測靈敏度。第二階段，調配不同鋁的比例做摻雜，電子載子濃度增加，有效提升感測催化能力，並找出最佳摻雜鋁的比例，做為此次非酵素葡萄糖感測電極並和第一階段的氧化鋅奈米柱做比較，第三階段使用第二階段最佳摻雜比例將其研製為光葡萄糖感測器。
藉由物性分析(掃描電子顯微鏡、X-射線繞射分析)，觀察其奈米結構形貌、元素含量，也更確切知道影響感測器之因素。另外，利用循環伏安法(CV)與電化學交流阻抗分析儀(EIS)觀察不同摻雜量下的氧化鋅奈米柱之電化學特性。藉由摻雜鋁元素改善後，量測在不同濃度下葡萄糖溶液(0~12 mM)與氫氧化鈉溶液(0.1 M)之循環伏安圖，再以最佳鋁摻雜發現具有高的靈敏度83.2(μA/cm2-mM)與決定係數(R2)0.993，第一階段分析氫氧化鈉濃度的不同提升了靈敏度與第二階段觀察到摻雜1.0%鋁原子會占據晶格間隙的位子，由於鋅原子與鋁原子半徑的不同而造成導致氧化鋅晶格的扭曲變形，使載子在晶界的散射增加導致霍爾移動率降低，造成體表面積下降造成導電率比摻雜0.5%鋁原子的略為上升使得靈敏度下降，摻雜0.5%的鋁原子有較適當的體表面積導電率最好使靈敏度最好，摻雜0.1%的鋁離子雖然有較高的體表面積摻雜過少的鋁離子使得導電度較差靈敏度最差，也藉由階段二階段摻雜最佳參數作為第三階段光葡萄糖感測器的研製，其靈敏度94.9(μA/cm2-mM)與決定係數(R2)0.994。

In this study, inorganic metal oxide semiconductors were used as the subject, and the glucose area was increased by the nanostructure method. This was used as the non-enzyme glucose sensing electrode, and the disadvantages of the enzyme electrode were improved and promote electrochemical detection the reaction sensitivity and stability of glucose.
The study was divided into three stages. The first-stage used a hydrothermal method to prepare a zinc oxide nanorods for comparative measurement of glucose sensing sensitivity under different concentrations of sodium hydroxide solution. In the second-stage, blend different aluminum ratios for doping that the concentration of electron carriers was increased and the sensing catalytic ability was effectively promoted. and the ratio of the best-doped aluminum is found that it as the non-enzymatic glucose sensing electrode and compared with the first-stage zinc oxide nanorods. The third-stage use optimal doping ratio in second stage to.develop an optical glucose sensor.
By physical property analysis (scanning electron microscopy and X-ray diffraction analysis), the nanostructured morphology and elemental content were observed, and the factors of effecting the sensor were more accurately known. In addition, electrochemical characteristics of zinc oxide nanorods at different doping amount were observed by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). After being improved by doping aluminum element, to measure the different concentration of glucose solution (0-12 mM) and sodium hydroxide solution (0.1 M) of cyclic voltammogram. It was found that the optimal aluminum doping have a high sensitivity of 83.2 (μA/cm2-mM) and a determination coefficient (R2) of 0.993. In the first-stage to analysis different concentration of sodium hydroxide to increase the sensitivity and observed in the second-stage that the doping 1.0% of aluminum atom would occupy the lattice gap due to the difference between the radius of zinc atoms and aluminum atoms that cause the distorted deformation of the crystal lattice of the zinc oxide, so that increase the scattering of the carrier at the grain boundary leads to a decrease in Hall mobility the Hall mobility decreases, and the decrease in the surface area causes the conductivity to be slightly higher than doping the 0.5% of aluminum atoms and the sensitivity is down, and doping 0.5% of aluminum atoms with the best of more appropriate body surface area conductivity and sensitivity. Although doping 0.1% of aluminum ions with a higher body surface area, a little amount of aluminum ions makes the poor conductivity and worst sensitivity. To make the three-stage light glucose sensor by stage-two doping optimal parameters that the sensitivity of 94.9 (μA/cm2-mM) and a determination coefficient (R2) of 0.994.

摘要 ⅰ
ABSTRACT ⅱ
誌謝 ⅳ
目錄 v
表目錄 vii
圖目錄 viii
第 1 章 緒論 1
1.1 前言 1
1.2 研究動機 2
1.2.1 糖尿病 2
1.2.2 酵素與非酵素型葡萄糖感測器 4
第 2 章 文獻回顧 5
2.1 何謂生物感測器 5
2.2 葡萄糖感測器歷史 6
2.2.1 第一型葡萄糖感測器 6
2.2.2 第二代葡萄糖感測器 7
2.2.3 第三代葡萄糖感測器 8
2.3 第四代非酵素型葡萄糖感測器 8
2.3.1 IHOAM 模型 8
2.3.2 Activated chemisorption model 10
2.3.3 金屬氧化物非酵素型葡萄糖感測器 10
2.4 電化學原理 11
2.4.1 電雙層電容器 13
2.4.2 三極式電化學量測系統 14
2.4.3 循環伏安法 15
2.4.4 Randles’等效模擬圖 (Randles’Equivalent Circuit) 16
2.4.5 電化學阻抗頻譜(Electrochemistry Impedance Spectroscopy, EIS) 17
2.5 氧化鋅基本結構與特性 19
2.6 AZO薄膜 21
2.7 摻雜金屬的優點 22
2.8 氧化鋅奈米結構成長機制 23
2.8.1 氣-液-固 (Vapor-Liquid-Solid, VLS)成長機制 23
2.8.2 氣-固 (Vapor-Solid, VS)成長機制 23
2.8.3 溶液-液-固(Solution-Liquid-Solid, SLS)成長機制 24
2.9 氧化鋅奈米結構合成方法 25
2.9.1 化學氣相沉積(Chemical Vapor Deposition, CVD) 25
2.9.2 物理氣相沉積(Physical Vapor Deposition, PVD) 26
2.9.3 水溶液法(Aqueous solution method) 26
2.9.4 水熱法(Hydrothermal method) 26
第 3 章 實驗方法 27
3.1 實驗儀器介紹 27
3.1.1 電化學分析儀器(Electrochemistry Workstation) 27
3.1.2 場發射掃描式電子顯微鏡(Field Emission Electron Microscope, FE-SEM) 27
3.1.3 高解析場發射穿透式電子顯微鏡(High-Resolution Transmission Electron Microscopy, HR-TEM) 28
3.1.4 X-射線繞射分析(XRD) 29
3.1.5 電子束蒸鍍機 (E-beam Evaporator) 31
3.1.6 射頻濺鍍機(RF sputtering) 32
3.2 玻璃基板清洗 33
3.3 電子束蒸鍍鉻、金層 34
3.4 氧化鋅晶種沉積 35
3.5 電化學量測系統 36
3.6 葡萄糖電解質溶液的調配 37
3.7 赤血鹽溶液的調配 37
3.8 氧化鋅實驗步驟 38
3.8.1 氧化鋅工作電極製作流程 38
3.8.2 低溫水熱法合成一維氧化鋅奈米結構 38
3.8.3 氧化鋅奈米結構製作葡萄糖感測器 40
3.9 氧化鋅不同鋁濃度摻雜實驗步驟 41
3.9.1 氧化鋅摻雜鋁工作電極製作流程 41
3.9.2 低溫水熱法合成一維鋁摻雜氧化鋅奈米結構 41
3.9.3 鋁摻雜氧化鋅奈米結構製作葡萄糖感測器 43
第 4 章 結果與討論 45
4.1 氧化鋅奈米柱結果討論 45
4.1.1氧化鋅奈米柱FE-SEM分析 45
4.1.2 氧化鋅奈米柱之電化學分析 46
4.2 鋁摻雜氧化鋅奈米柱結果討論 54
4.2.1 不同鋁摻雜氧化鋅奈米柱之FE-SEM分析 54
4.2.2 氧化鋁鋅奈米奈米柱之循環伏安法量測 56
4.2.3 氧化鋁鋅奈米柱之穩定性量測 59
4.3 氧化鋁鋅光葡萄糖感測器 70
4.3.1 光檢測器薄膜測試 70
4.3.2 氧化鋁鋅奈米柱UV光與暗電流之循環伏安法量測 72
4.2.3 AZO NRs 非酵素葡萄糖感測器能帶圖 74
第 5 章 結論 76
參考文獻 77
Conference 84

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