臺灣博碩士論文加值系統

本研究成功製備二維層狀過渡金屬硫化物修飾氧化亞銅/氧化鋅奈米柱複合電極於Ex-ITO(耐高溫)玻璃上，利用兩段式加熱成長二硫化鉬具有製程簡化、反應快、成本低與接觸面積大等優點，將其應用於非酵素型葡萄糖感測器中。製程主要分為三個部分：第一部份為在Ex-ITO玻璃上濺鍍晶種層並成長氧化鋅奈米柱，藉由退火調整表面平整度並探討水熱法製程時間2小時至4小時之對應柱長；第二部分為預鍍金屬硫化法沉積二硫化鉬於氧化鋅奈米柱上，透過磁控濺鍍系統分別以濺鍍時間1、3、5、10秒成長鉬薄膜，並根據硫熔點113℃進行兩段式加熱得到片狀二硫化鉬；第三部分為利用電化學沉積氧化亞銅於二硫化鉬/氧化鋅奈米柱形成異質結構，材料間協同效應使氧化亞銅形成奈米顆粒並沉積於電極表面，調整電鍍時間控制其覆蓋比例提高表面積；最後是量測方面，透過冷場發射掃描式電子顯微鏡(FE-SEM)觀測不同結構之表面形貌，光柵光譜儀(UV-vis)與拉曼光譜儀(Raman shift)觀察薄膜沉積狀況與材料特徵峰值，以X光繞射儀(XRD)配合高解析度穿透式電子顯微鏡(HRTEM)觀察材料之結晶方向與橫截面型貌，利用X射線光電子能譜儀(XPS)測定其元素構成與表面化學能譜，最後透過電化學儀檢測各種感測器特性。
實驗結果顯示，氧化鋅奈米柱在水熱法中的最佳成長時間為2小時，二硫化鉬濺鍍時間為3秒，硫化溫度為640度，氧化亞銅電鍍時間為90秒之複合電極，在0.1 M濃度之NaOH中逐步提升葡萄糖濃度(0-200mg/dL)進行電化學循環伏安法(Cyclic Voltammetry, CV)，對比於未加入MoS2之複合電極，其靈敏度自396提升至680.4 ，R2(擬合優越度)值分別為0.985、0.993。透過計時電流法(chronoamperometry)可得到兩個線性區間，分別518.3 (0-5.556 mM)以及233.9 (5.556 mM-11.11mM)，其R2值分別為0.993與0.987。

This study successfully fabricated two-dimensional layered transition metal sulfide-modified Cu2O/ZnO nanorod composite electrodes on Ex-ITO (high-temperature resistant) glass. By using a two-step heating process, MoS2 was grown, simplifying the process and offering advantages such as rapid reaction, low cost, and large contact area. This composite was applied to non-enzymatic glucose sensors. The fabrication process mainly consisted of three parts: 1. Sputtering a seed layer on Ex-ITO glass and growing ZnO nanorods, with annealing to adjust surface smoothness and investigating the effect of hydrothermal process times ranging from 2 to 4 hours on the corresponding rod length. 2. Depositing MoS2 on ZnO nanorods using a pre-deposition sulfide method. A magnetron sputtering system was used to grow Mo thin films with sputtering times of 1, 3, 5, and 10 seconds, and a two-step heating process based on sulfur's melting point of 113℃ was applied to obtain sheet-like MoS2. 3. Electrochemically depositing Cu2O on the MoS2/ZnO nanorods to form a heterostructure. The synergistic effect among the materials led to the formation of Cu2O nanoparticles deposited on the electrode surface. Adjusting the electroplating time controlled the coverage ratio and increased the surface area.
Regarding measurement, different structural surface morphologies were observed using field emission scanning electron microscopy (FE-SEM). UV-visible spectroscopy and Raman spectroscopy were used to observe the film deposition status and material characteristic peaks. X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) were used to observe the crystalline orientation and cross-sectional morphology of the materials. X-ray photoelectron spectroscopy (XPS) was employed to determine the elemental composition and surface chemical spectra. Finally, various sensor characteristics were detected using an electrochemical analyzer.
The experimental results showed that the optimal growth time for ZnO nanorods in the hydrothermal method was 2 hours, the sputtering time for MoS2 was 3 seconds, the sulfidation temperature was 640℃, and the electroplating time for Cu2O was 90 seconds. The composite electrode was tested in 0.1 M NaOH with gradually increasing glucose concentrations (0-200 mg/dL) using cyclic voltammetry (CV). Compared to the composite electrode without MoS2, its sensitivity increased from 396 to 680.4 , and the R2 (goodness of fit) values were 0.985 and 0.993, respectively. Chronoamperometry revealed two linear ranges, 518.3 (0-5.556 mM) and 233.9 (5.556 mM-11.11 mM), with R2 values of 0.993 and 0.987, respectively.

摘要 i
ABSTRACT iii
誌謝 v
目錄 vi
表目錄 x
圖目錄 xi
第一章　緒論 1
1-1 前言 1
1-2 研究動機 6
1-3 研究方法 8
第二章　文獻回顧 9
2-1 感測器簡介 9
2-2 葡萄糖生物感測器 10
2-3-1 酵素型葡萄糖感測器 11
2-3-2 非酵素型葡萄糖感測器 13
2-3 二維材料 16
2-3-1 二維材料簡介 16
2-3-2 二硫化鉬(Molybdenum Disulfide, MoS2) 21
2-3-3 製備MoS2 24
2-3-4 基於MoS2的非酵素型葡萄糖感測器 30
2-4 氧化鋅奈米柱 32
2-4-1氧化鋅簡介 32
2-4-2氧化鋅合成方式 33
2-5 氧化亞銅 36
第三章　實驗方法與步驟 38
3-1 實驗藥品及耗材 38
3-2 實驗架構及流程圖 39
3-3 實驗步驟及方法 41
3-3-1 基板選擇與處理 41
3-3-2 製備氧化鋅晶種層 42
3-3-3 熱退火處理 44
3-3-4 水熱法合成氧化鋅奈米柱 45
3-3-5 利用濺鍍系統沉積鉬金屬 46
3-3-6 利用熱蒸氣硫化成長二硫化鉬 48
3-3-7 電鍍沉積氧化亞銅 50
3-3-8 奈米碳管固定劑調配與感測器製作 53
3-4 分析儀器介紹 54
3-4-1 光學顯微鏡 (Optical Microscopy, OM) 54
3-4-2 冷場發射掃描式電子顯微鏡(FE-SEM) 55
3-4-3 X光繞射儀(X-ray diffraction, XRD) 56
3-4-4 拉曼光譜儀(Raman spectrometer) 58
3-4-5 多功能聚焦離子束系統 (Focused Ion Beam, FIB) 60
3-4-6 高解析度穿透式電子顯微鏡(HRTEM) 61
3-4-7 X射線光電子能譜儀(X-ray photoelectron spectroscopy) 62
3-4-7 光柵光譜儀(UV/Visible Spectrophotometer) 63
3-4-8 電化學分析儀(Electric chemistry analyzer) 65
第四章　結果與討論 67
4-1 氧化鋅晶種層與氧化鋅奈米柱之製備 67
4-1-1 光柵光譜儀分析氧化鋅晶種層與氧化鋅奈米柱 67
4-1-2 Raman 光譜分析 70
4-1-3 氧化鋅奈米柱之SEM表面形貌 72
4-1-4 X光繞射儀(X-ray diffraction, XRD) 76
4-2 鉬金屬硫化形成二硫化鉬(MoS2)/氧化鋅奈米柱(ZnO NRs) 78
4-2-1 以光學顯微鏡觀察二硫化鉬薄膜 78
4-2-2 UV–vis 分析二硫化鉬/氧化鋅奈米柱 79
4-2-3 Raman 光譜分析 81
4-2-4 二硫化鉬/氧化鋅奈米柱之SEM表面形貌 83
4-2-5 X光繞射儀(X-ray diffraction, XRD) 87
4-2-6 高解析度穿透式電子顯微鏡(HRTEM) 88
4-3 氧化亞銅(Cu2O)/二硫化鉬(MoS2)/氧化鋅奈米柱(ZnO NRs)複合電極 89
4-3-1 製備氧化亞銅於ITO玻璃 89
4-3-2 Raman 光譜分析 91
4-3-3 SEM分析氧化亞銅/二硫化鉬/氧化鋅奈米柱其表面形貌 92
4-3-4 X光繞射儀分析(X-ray diffraction, XRD) 95
4-3-5 高解析度穿透式電子顯微鏡(HRTEM) 96
4-3-6 X射線光電子能譜儀(X-ray photoelectron spectroscopy) 98
4-4 電化學儀量測非酵素葡萄糖感測器 101
4-4-1 循環伏安法(Cyclic Voltammetry, CV) 101
4-4-2 計時電流法(chronoamperometry, CA) 104
4-4-3 抗干擾與穩定性測試 106
4-4-4 葡萄糖感測器性能比對 108
第五章　結論 109
參考文獻 111

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