臺灣博碩士論文加值系統

第一部份：在本研究中，利用簡單、環保的水熱法，來製備多孔性質的石墨碳氮化物/二氧化錳奈米複合材料（GCN / MnO2），將它修飾於絲網印刷碳電極（Screen printed carbon electrode，SPCE），並首次應用於亞硝酸鹽的電化學檢測，該奈米複合材料電極快速且靈敏的檢測效能，有助於亞硝酸鹽電化學檢測上的發展。此實驗中，採用各種物理化學技術檢測性質：X射線繞射分析（XRD），傅里葉轉換紅外光譜（FT-IR），X-射線光電子光譜（XPS），N2吸附-脫附等溫線，場發射掃描式電子顯微鏡（FE-SEM）和高解析場發射穿透式電子顯微鏡（HR-TEM）對其形貌和結構性質進行了驗證；再來使用循環伏安法（CV）、電化學阻抗光譜（EIS）和微分脈衝伏安法（DPV）中，研究了石墨氮化物/二氧化錳修飾絲網印刷碳電極，對亞硝酸鹽的氧化還原性能。在研究中顯示，GCN / MnO2修飾電極具有高靈敏度¬(24.1777 μA µM-1 cm-2)、低檢測限(1.23 nM)，以及線性範圍廣(0.01–1520 μm)，並且在實際樣品 (腐爛牛肉、自來水、飲水機過濾水)的檢測中，顯示良好的電催化特性，同時具有良好的抗干擾性質，這代表其具有高度實用的價值，可應用於食品安全相關的檢測上。

第二部份：本研究中，先使用簡單的水熱法，合成二硫化鎳/氧化石墨烯（NiS2 / GO）的奈米複合材料，並修飾玻璃探電極，進一步用於檢測毒性物質4-羥基硝基苯（4-HNB）的電化學感測中。在實驗中，通過X射線繞射（XRD）、X-射線光電子光譜（XPS）先確定奈米材料的基團，再使用高解析場發射穿透式電子顯微鏡（HR-TEM）對奈米複合材料的外觀進行研究；接著也利用循環伏安法（CV）、微分脈衝伏安法（DPV）來驗證二硫化鎳/氧化石墨烯修飾玻璃探電極(NiS2 / GO-GCE)的電化學性能，與未修飾的玻璃碳電極(GCE)相比，該電極對於4-HNB的感測性能非常顯著，同時測出的感測器具有寬廣線性範圍(0.1000-1053 μM)，和極低的檢測極限(59.5 nM)。另一方面，真實河水樣品的檢測，也有96%以上的檢出率，這表示NiS2 / GO-GCE非常適合應於真實水質的毒物檢測中。

Part I：In this study, a simple and environmentally friendly hydrothermal method was used to prepare a porous graphite carbonitride/manganese dioxide nanocomposite (GCN/MnO2), which was modified on a screen printed carbon electrode(SPCE), and for the first time applied to the electrochemical detection of nitrite, the rapid and sensitive detection efficiency of the nanocomposite electrode is helpful for the development of nitrite electrochemical detection. In this experiment, various physical and chemical techniques were used to detect properties: X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), N2 adsorption-desorption isotherm Field emission scanning electron microscopy (FE-SEM) and high-resolution field emission transmission electron microscopy (HR-TEM) were used to verify its morphology and structural properties, using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and differential pulse voltammetry (DPV), graphite nitride/manganese dioxide modified screen-printed carbon electrodes were studied for nitrite redox performance. In the study, GCN / MnO2 modified electrodes have high sensitivity (24.1777 μA μM-1 cm-2), low detection limit (1.23 nM), and a wide linear range (0.01–1520 μm), and in actual samples (rotation) In the detection of beef, tap water and water filter, it shows good electrocatalytic properties and good anti-interference properties, which means it has high practical value and can be applied to food safety related testing.

Part II：In this study, a simple hydrothermal method was used to synthesize a nickel-nickel oxide/graphene oxide (NiS2 / GO) nanocomposite, and a glass probe was modified to further detect the toxic substance 4-hydroxynitrobenzene (4-HNB) in electrochemical sensing. In the experiment, the groups of the nanomaterials were first determined by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), and then the high-resolution field emission transmission electron microscope (HR-TEM) was used to laminate the nano composites. The appearance of the study; Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were also used to verify the electrochemical performance of nickel disulfide/graphene oxide modified glass probe (NiS2 / GO-GCE) with unmodified glassy carbon. Compared to the electrode (GCE), the sensor's sensing performance for 4-HNB is very significant, while the measured sensor has a wide linear range (0.1000-1053 μM) and a very low detection limit (59.5 nM). On the other hand, the detection of real river water samples also has a detection rate of more than 96%, which means that NiS2 / GO-GCE is very suitable for the detection of poisons in real water quality.

摘要 i
ABSTRACT iii
致謝 v
目 錄 vi
表目錄 ix
圖目錄 x
第一章 緒論 1
1.1　電化學簡介 1
1.2　電化學分析簡介 1
1.3　修飾電極簡介 2
1.4　材料簡介 3
1.4.1　亞硝酸鹽 3
1.4.2　二氧化錳 4
1.4.3　二硫化鎳 5
1.4.4　對硝基苯酚 5
1.4.5　氧化石墨烯 5
第二章 　實驗藥品、器材和分析法 7
2.1.　實驗藥品簡介 7
2.2.　實驗器材 8
2.3.　分析方法 13
2.3.1.　循環伏安法(Cyclic voltammetry，CV) 13
2.3.2.　掃描式電子顯微鏡(Scanning Electron Microscope，SEM) 14
2.3.3.　微分脈衝伏安法(Differential Pulse Voltammetry，DPV) 14
2.3.4.　X-射線繞射分析(X-ray Diffraction，XRD) 15
2.3.5.　比表面積檢測法(Brunauer-Emmett-Teller Theory ) 17
2.3.6.　電化學阻抗光譜(Electrochemistry Impedance Spectroscopy，EIS) 18
2.3.7.　傅里葉轉換紅外光譜 （Fourier-transform infrared spectroscopy，FTIR） 18
第三章 　石墨氮化物/二氧化錳修飾絲網印刷碳電極用於亞硝酸鹽電化學檢測 19
3.1　前言 19
3.2　實驗步驟 20
3.2.1　GCN與GCN / MnO2的合成 20
3.2.2　GCN / MnO2修飾電極的製備 21
3.3　實驗結果與討論 22
3.3.1　GCN / MnO2奈米複合材料的結構性能 22
3.3.2　電化學性能研究 29
3.3.3　GCN / MnO2奈米複合材料對亞硝酸根的電催化作用 31
3.3.4　亞硝酸鹽的測定 33
3.3.5　穩定性、重複性和再現性 35
3.3.6　真實樣品分析 36
3.4　結論 37
第四章 　二硫化鎳/氧化石墨烯修飾玻璃碳電極在河水中檢測4-羥基硝基苯 38
4.1 前言 38
4.2 實驗步驟 40
4.2.1 NiS2 材料的合成 40
4.2.1 NiS2 / GO - GCE修飾電極的製備 40
4.3 實驗結果與討論 41
4.3.1 結構和形態特徵 41
4.3.2 電化學性能研究 44
4.3.3 酸鹼值的反應 47
4.3.4 4-HNB的伏安法測定 49
4.3.5 感測器的穩定性和再現性 51
4.3.6 實際樣本分析 51
4.4 結論 52
參考資料 53

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