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研究生： 林立紘
Lin, Li-Hung
論文名稱： 電化學製備金/氧化鎳/泡沫銅電極應用於非酶葡萄糖傳感器
Electrochemical Preparation of Gold and Nickel Oxide Modified Copper Foam Electrode for Non-enzymatic Glucose Sensor
指導教授： 黃守仁
Whang, Thou-Jen
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2023
畢業學年度： 111
語文別： 中文
論文頁數： 89
中文關鍵詞： 葡萄糖 、泡沫銅 、氧化鎳 、電催化
外文關鍵詞： glucose, copper foam, nickel oxide, electrocatalysis
相關次數： 點閱：103  下載：8 
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    • 本研究使用具有高比表面積、低毒性之三維開孔結構泡沫銅( Open-cell Copper foam, CF )作為金屬骨架，利用定電位法沉積並鍛燒形成島狀NiO，再通過電化學置換於表面修飾Au。將製備而成之Au/NiO/CF電極應用於電催化葡萄糖氧化反應。
    通過調控前處理方式，以及Ni(NO3)2沉積時間、電位、濃度；鍛燒時間、溫度、方式；電置換HAuCl4 溶液濃度、時間等參數。並利用掃描式電子顯微鏡 (SEM)、能量色散X射線光譜(EDS)、X射線繞射分析儀器(XRD)等儀器，對各參數進行表面形貌及元素組成、晶體結構。配合循環伏安法(CV)，進行催化葡萄糖氧化之效果分析。並取得最佳化製備條件為使用甲醇、去離子水依序進行10分鐘超音波震盪前處理後，於0.1 M硝酸鎳溶液中進行定電位沉積，固定電位為-1.0 V (vs Ag/AgCl)，沉積時間為 300秒。並進行250°C空氣鍛燒1.5小時。最終浸泡於10 mM HAuCl4溶液10秒，即完成Au/NiO/CF電極。
    經由SEM、EDS mapping、XRD等儀器鑑定所製備電極特徵，並利用最佳化條件Au/NiO/CF電極進行葡萄糖之感測，於電催化葡萄糖氧化方面，與僅通過前處理泡沫銅電極相比，展現出較良好的傳感特性。工作電位為0.4 V時，線性範圍為 0.07 mM ~ 0.84 mM ( ip = 0.0004[Glucose] + 0.0002，R² = 0.9964 )。偵測極限LOD為0.421 μM。

    In this study, a three-dimensional Open-Cell Copper Foam (CF) with high specific surface area and low toxicity was used as the metal frame, deposited and calcined by a constant potential method to form island-like NiO, and then modified Au by galvanic replacement on the surface. The prepared Au/NiO/CF electrode was applied to electrocatalyze the oxidation of glucose.
    By adjusting the pretreatment method and Ni(NO3)2 deposition time, potential, concentration; calcination time, temperature, method; electro-displacement HAuCl4 solution concentration, time and other parameters. And using Scanning Electron Microscope (SEM), Energy Dispersive X-ray Spectroscopy (EDS), X-ray Diffraction analysis instrument (XRD) and other instruments, combined with Cyclic Voltammetry (CV) to analyze the surface morphology and elemental composition of each parameter, analysis of the crystal structure and the effect of catalyzing the oxidation of glucose. The optimal preparation conditions were obtained as follows, methanol and deionized water were used for 10 minutes of ultrasonic shock pretreatment. Then, the constant potential deposition was carried out in 0.1 M nickel nitrate solution, and the fixed potential was -1.0 V (vs Ag/AgCl) with a deposition time of 300 seconds. And carry out 250°C air calcination for 1.5 hours. Finally soak in 10 mM HAuCl4 solution for 10 seconds to complete the Au/NiO/CF electrode.
    The characteristics of the prepared electrode were identified by SEM, EDS mapping, XRD and other instruments, and the optimized condition Au/NiO/CF electrode was used for glucose sensing. In terms of electrocatalytic glucose oxidation, compared with only pre-treated foam copper electrode, showing better sensing properties.
    When using the working potential at 0.4 V, with a linear range of 0.07 mM ~ 0.84 mM. (ip = 0.0004[Glucose] + 0.0002, R² = 0.9964), a sensitivity of 410.99 μA mM−1, a low limit of detection (LOD) of 0.421 μM. (S/N = 3)

    摘要 I 致謝 XV 目錄 XVI 圖目錄 XIX 表目錄 XXIII 第一章 緒論 1 1-1 研究動機 1 1-2 葡萄糖傳感器 2 1-2-1 酶類葡萄糖傳感器 2 1-2-2 非酶葡萄糖傳感器 5 1-3 泡沫銅 (Copper Foam, CF) 6 1-4 氧化鎳 (Nickel(II) oxide, NiO) 7 1-5 研究目的 8 第二章 實驗原理與儀器原理 9 2-1 實驗原理 9 2-1-1 電化學原理 9 2-1-2 電化學沉積氧化鎳機制 12 2-1-3 電化學置換(Galvanic Replacement Reaction, GR)沉積金機制 12 2-1-4 氧化鎳催化葡萄糖氧化機制 13 2-1-5 金催化葡萄糖氧化機制 14 2-1-6 金/氧化鎳催化葡萄糖氧化機制 15 2-1-7 鍛燒薄膜固態除潤(solid-state dewetting)機制 17 2-2 儀器原理 19 2-2-1 掃描式電子顯微鏡 (Scanning electron microscope, SEM) 19 2-2-2 能量色散X射線光譜(Energy-dispersive X-ray spectroscopy, EDS) 21 2-2-3 X射線繞射分析儀器(X-ray Diffractometer, XRD) 22 第三章 儀器設備與實驗方法 23 3-1 實驗流程 23 3-2 實驗儀器 24 3-3 實驗藥品及材料 25 3-4 實驗方法: 26 3-4-1 Au/NiO/CF電極之製備 26 3-5 電化學方法感測葡萄糖 27 第四章 結果與討論 28 4-1 Au/NiO/CF電極製備條件最佳化 28 4-1-1 前處理對泡沫銅表面形貌探討 28 4-1-2 Ni(NO3)2沉積時間之影響 31 4-1-3 Ni(NO3)2沉積電位之影響 36 4-1-4 Ni(NO3)2濃度之影響 41 4-1-5 鍛燒時間之影響 45 4-1-6 鍛燒溫度之影響 48 4-1-7 鍛燒方式之影響 51 4-1-8 電置換HAuCl4濃度、時間之影響 52 4-2 最佳化製備條件Au/NiO/CF結構鑑定圖 61 4-3 探討Au/NiO/CF電極對葡萄糖之電化學行為 67 4-4 電化學感測葡萄糖 69 4-4-1 葡萄糖傳感器工作電位探討 69 4-4-2 葡萄糖濃度之感測 72 4-4-3 干擾物之檢測 77 4-4-4 穩定性之檢測 78 第五章 結論 80 參考文獻 82

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