臺灣博碩士論文加值系統

本研究以金、銀奈米粒子修飾氧化亞銅之摻鋁氧化鋅(AZO)奈米柱複合材料在ITO玻璃，成功應用在非酵素葡萄糖感測中。實驗主要將分為四個部分：第一部份為在製鍍不同厚度之AZO晶種層，經水熱法成長AZO奈米柱陣列，再透過掃描式電子顯微鏡(SEM)與X光繞射儀(XRD)分析最佳晶種層；第二部分電化學沉積氧化亞銅於AZO奈米柱上，測得最適合對氧化亞銅沈積的AZO奈米柱最佳參數，以X光光電子能譜儀對氧化亞銅沈積之電解液pH值進行氧化態分析，測得最佳沈積時間；第三部分為化學合成金、銀奈米粒子，利用UV-Vis吸收光譜與SEM測得最佳粒徑，並透過Nafion分散均勻滴覆在Cu2O/AZO NR表面測定最佳靈敏度、線性度與擬合優越度；最後以電化學量測分析其氧化還原反應特性。
葡萄糖濃度0、50、100、150、200 (mg/dL)符合人體血糖濃度進行電化學儀的循環伏安法(CV)，在Cu2O/AZO NR/ITO複合材料上對濃度與電流關係做線性擬合，得到其斜率為26.117、擬合優越度R2為0.9424。利用Nafion分散金、銀奈米粒子的作用下，將奈米粒子分佈在感測器表面幫助介面穩定，在金奈米修飾下測得其斜率變化提升至27.456，R2值達0.9643。
透過計時安培法(CA)量測在實際濃度變化時電流反應，在電位0.6 V環境下以銀奈米修飾電極測得最佳靈敏度12.3 (221.6 )，其線性範圍達60 – 200 mg/dL (3.33 – 11.11 mM)，擬合度R2達0.997，可準確用於人體血糖感測。

The research is about using precious metal nanoparticles modified Cu2O/AZO composite on ITO glass ,and successfuly applied in non-enzymatic Glucose Sensor.
There’re four parts of the experiment: First, coating different thickness of Aluminum-doped Zinc Oxide (AZO) seed layer for growing AZO nanorod arrays by hydrothermal method, then using SEM and XRD analyzed the best seed layer parameter. Second, electrodepositing Cuprous oxide (Cu2O) on AZO nanorod, and measured the best parameter for deposited Cu2O on AZO nanorods, then using XPS to analyze the Oxidation state of pH value in Cu2O precursor solution, and measuring the best deposition time. Third, chemical synthesis Au, Ag nanoparticles, and using UV-Vis absorption spectrum and SEM to get the best particle size, also through the Nafion to evenly dispersed on the surface of Cu2O/AZO NR, Last, analyzing its’ Redox reactions characteristic through the electrochemical analyzer, and also the best sensitivity, linearity and accuracy.
Selecting the concentration of glucose 0, 50, 100, 150, 200 (mg/dL) which are match the human blood glucose to do the Cyclic voltammetry (CV) of electrochemical analyzer. Then linear fitting the relation of concentration and current on Cu2O/AZO NR/ITO composite to get its’ change slope is 26.117 and the coefficient of determination (R2 ) is 0.9424. Using Nafion to disperse Au, Ag nanoparticles to let the nanoparticles spread on the surface of sensor for helping its’ interface be stable, the slope increased to 27.456 and the R2 is up to 0.9643 by modified with Au nanoparticles.
To measure the reaction of current in changing concentration through the Chronoamperometry (CA) ,when working potential in 0.6V can get the best sensitivity in 12.3 (221.6 ) with modified by Ag nanoparticle, and the linear range is to 60 – 200 mg/dL (3.33 – 11.11 mM) and the R2 is up to 0.997, thus, it’s suit to sense blood sugar of human body.

摘要 i
ABSTRACT ii
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 4
1-3 論文架構 5
第二章　理論探討與文獻回顧 6
2-1 感測器簡介 6
2-1-1 感測器種類 7
2-2 摻鋁氧化鋅(AZO) 12
2-2-1 摻鋁氧化鋅特性 12
2-2-2 摻鋁氧化鋅奈米柱合成方式[25-28] 13
2-3 氧化亞銅 18
2-4 貴金屬奈米粒子 19
2-5 文獻回顧 20
第三章　實驗方法與步驟 24
3-1 實驗流程 24
3-2 實驗藥品及耗材 27
3-3 儀器設備介紹 28
3-3-1 冷場發射掃描式電子顯微鏡(Cold Field Emission Scanning Electron Microscope, FE-SEM) 28
3-3-2 UV-可見光光柵光譜儀(UV-Visible Spectrophotometer) 29
3-3-3 X光繞射儀(X-ray diffraction, XRD) 30
3-3-4 拉曼光譜儀(Raman spectrometer) 32
3-3-5 X射線光電子能譜儀(X-ray photoelectron spectroscopy) 33
3-3-6 電化學分析儀(Electric chemistry analyzer) 34
3-4 實驗步驟及方法 36
3-4-1 基板清洗 36
3-4-2 網版印刷電極 37
3-4-3 製備摻鋁氧化鋅(AZO)晶種層 38
3-4-4 水熱法合成摻鋁氧化鋅(AZO)奈米柱 41
3-4-5 氧化亞銅沈積 42
3-4-6 金/銀奈米粒子調配 44
3-4-7 Nafion 固定劑調配 45
第四章　結果與討論 46
4-1 摻鋁氧化鋅(AZO)奈米柱 46
4-1-1 AZO晶種層特性分析 46
4-1-2 XRD探討AZO奈米柱結晶狀態 51
4-2 氧化亞銅沈積特性探討 52
4-2-1 Raman光譜分析氧化亞銅沈積情形 55
4-2-2 XPS能譜分析沈積情形 56
4-2-3 Cu2O/AZO奈米柱表面形貌 59
4-2-4 XRD探討Cu2O在AZO奈米柱沈積情形 62
4-3 貴金屬奈米粒子 63
4-3-1 奈米粒子形貌分析 63
4-3-2 SEM探討奈米粒子 66
4-4 電化學特性量測分析 68
4-4-1 氧化還原電位範圍 68
4-4-2 循環伏安法(CV)曲線分析 70
4-4-3 以金屬奈米粒子修飾Cu2O/AZO NR感測電極試片 76
4-5 計時電流滴定量測(Chronoamperometry) 79
4-5-1 反應工作電位 79
4-5-2 金屬奈米粒子修飾計時電流量測 81
4-5-3 相關電流式感測器文獻比較 87
第五章　結論 88
參考文獻 90

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