臺灣博碩士論文加值系統

第一部分
甲基對氧磷（MOX）是一種劇毒的有機磷酸鹽農藥。有報導指出，MOX可透過攝取、吸入或皮膚滲透進入人體。由於其高度不可降解性，它可以輕易地與水果和蔬菜的組織結合，當甲基對氧磷（MOX）被消耗時，它可以透過抑制人體新陳代謝中的乙醯膽鹼酯酶使得亞慢性和慢性疾病加重，所以我們首次研究了以三維結構(3D)多孔相(porous phase)氧化石墨烯包覆黃銅礦(CuFeS2)的奈米複合材料(GOS@CuFeS2)的非酶電化學感測器檢測，因此，在開發用於農藥可靠的即時檢測感測器，必須克服傳統方法中實際遇到的限制。在網板印刷碳電極鍍上一層(GOS@CuFeS2)奈米複合材料薄膜對MOX具有出色的電催化性能，在優化的工作條件下，修飾電極提供的線性響應範圍是0.073至801.5µM、檢測極限為4.5nM，此感測器出色的靈敏度為17.97 µA µM–1cm–2。此複合材料可以用於電催化上有前景的電極調節劑。最後，(GOS@CuFeS2)奈米複合材料修飾電極在蔬菜實際樣品中顯示出更高的即時使用性。
第二部分
我們透過一步驟合成法合成出B / N共摻雜中孔洞碳材料（BNDC），可以用於異煙鹼醯聯胺（INZ）的高靈敏度電化學檢測。該合成方法簡單，並且產生具有高度元素純度和中孔表面的均勻摻雜原子。此外，透過氮氣（N2）吸附-脫附分析和光譜研究來分析合成後BNDC的表面和物理化學性質。BNDC薄膜修飾電極對INZ具有高靈敏度的感測及出色的分析能力，工作濃度範圍為0.02-1783 µM；檢測極限是1.5 nM。
此合成出來的BNDC感測器優點是具有廣大催化表面積、低孔徑、豐富活性點位和優異電導度。此外，BNDC優異的化學穩定性提供了電化學測定時的長期穩定性和再現性，透過檢測生理流體中的INZ來評估所設計出的感測器實用性。
第三部分
全球最大的金屬鋁生產國家近期宣布將於2019年中封鎖境內各地金屬鋁的生產，以盡量減少冬季空氣污染。這些報告促使人們意識到金屬鋁的回收再利用是有必要性的，我們透過一步驟超聲化學法回收了氧化鋁奈米粒子(Al2O3 NPs)，透過FE-SEM和TEM檢測Al2O3奈米粒子的結構形態；以及使用XPS和XRD分析驗證回收的Al2O3 NPs的純度。將回收的Al2O3 NPs應用於奧美拉唑omeprazole (OMZ)的檢測中，在良好優化條件下，圖中繪製的校準曲線是在Al2O3 NPs/GCE下對OMZ檢測所獲得的，其具有0.025-433.3μM的寬大線性濃度範圍，最小偵測極限為9.1 nM。所以近期此回收材料被積極應用於超級電容器上，其在1M KOH下在1A / g電流密度下表現出明顯的比電容值（688F / g），並且即使在3000GCD循環後仍保持86%的電容保持率。

Part 1
Methyl paraoxon (MOX) is a highly toxic organophosphate pesticide. It is recently reported that, MOX can enter the human body through ingestion, inhalation, or by dermal penetration. Due to its high non-degradability, it can bind to the tissues of fruits and vegetables. When it is consumed, it can imposes sub-chronic and chronic diseases, by the inhibition of acetylcholinesterase in human metabolism. Therefore, for the first time, we reported a detection of non-enzymatic electrochemical sensor based on 3D porous phase graphene oxide sheets encapsulated chalcopyrite (GOS@CuFeS2) nanocomposite. Hence, the development of reliable sensors for the real-time detection of pesticides is imperative to overcome practical limitations encountered in conventional methodologies. As synthesized GOS@CuFeS2 nanocomposite film screen-printed carbon modified electrode (SPCE) displays excellent electrocatalytic ability towards MOX. Under optimized working conditions, the modified electrode provides linear response range from 0.073 to 801.5 μM. The detection limit was obtained as 4.5 nM. The sensor displayed outstanding sensitivity as 17.97 µA µM–1 cm–2. This composite could be a promising electrode modifier for electrocatalysis. Finally, the GOS@CuFeS2 nanocomposite modified electrode shows greater real-time practicality in vegetable real samples. The obtained moral parameters from the developed method were compared with the authenticated HPLC results.
Part 2
At present, B/N co-doped mesoporous carbon (BNDC) have been synthesized in one-step and employed for high sensitive electrochemical detection of Isoniazid (INZ). The synthetic procedure was simple and produced homogenous doping of heteroatoms with high elemental purity, and mesoporous surface. Further, the surface and physiochemical properties of synthesized BNDC was analysis by Nitrogen (N2) adsorption-desorption analysis, and spectroscopic studies. A high sensitive amperometric sensor of BNDC film modified electrode, towards INZ, delivered superior analytical performance with a broad dynamic range 0.02–1783 µM and detection limit of 1.5 nM. Excellency of electrochemical sensor can be attributed to the large surface area, low pore size, abundant active sites, and enhanced electrical conductivity of synthesized BNDC electrocatalyst. Furthermore, the excellent chemical stability of BNDC advocate the long-term stability and reproducibility of the fabricated electrochemical assay. The practical applicability of the proposed sensor was assessed by detection of INZ in physiological fluids.
Part 3
The world’s largest aluminium producer has publicized that will blockout aluminum production all over the country from November 2018 to March 2019, in order to minimize winter air pollution. Presumably, these sort of reports urge the chemists to perceive that recovery or recycle of aluminum is decisive. In this article, our group has recovered aluminium oxide nanoparticles (Al2O3 NPs) through a facile one-step sonochemical methodology. The morphological details of Al2O3 NPs were examined by FE-SEM and TEM; finally, the purity of as-recovered Al2O3 NPs were confirmed by XPS and XRD. The as-recovered Al2O3 NPs were employed for the specific and sensitive detection of omeprazole (OMZ), which comes under the class of proton-pump inhibitor. Under the well-optimized conditions, the graphically plotted calibration curve was attained at Al2O3 NPs/GCE towards the detection of OMZ, which possesses the wider linear range of 0.025-433.3 µM, with the minimal detection limit of 9.1 nM. Furthermore, the recovered material was employed as an active participant in supercapacitor application, which exhibited an appreciable specific capacitance value (688 F/g) at 1 A/g current density in 1 M KOH and maintained 86% capacitance retention even after 3000 GCD cycles.

摘　要 i
ABSTRACT iii
致 謝 vi
目錄 vii
表目錄 x
圖目錄 xi
第一章 緒論 1
1.1 電化學簡介 1
1.2 感測器之定義 3
1.2.1 生物感測器 4
1.3 電極 7
1.3.1 化學修飾電極簡介 7
1.4 藥品簡介 9
1.4.1 甲基對氧磷(Paraoxon-Methyl) (Paraoxon) 9
1.4.2 氧化石墨烯懸浮液(Graphene Oxide Suspension,GOS) 9
1.4.3 半胱氨酸L-cysteine (C3H7NO2S) 10
1.4.4 異煙肼(Isoniazid) 11
1.4.5 過硫酸銨(Ammonium persulfate , APS) 12
1.4.6 奧美拉唑(Omeprazole , OMZ) 13
第二章 實驗藥品、器材與分析方法 14
2.1 實驗藥品 14
2.2 實驗器材 15
2.3 分析方法 16
2.3.1 循環伏安法(Cyclic Voltammetry，CV) 16
2.3.2 微分脈衝伏安法 (Differential Pulse Voltammetry，DPV) 17
2.3.3 電化學阻抗譜(Electrochemical Impedance Spectroscopy， EIS) 18
2.3.4 掃描式電子顯微鏡(Scanning Electron Microscope，SEM) 20
2.3.5 穿透式電子顯微鏡(Transmission Electron Microscopy，TEM) 22
2.3.6 X-射線繞射分析儀(X-ray Diffractometer，XRD) 24
2.3.7 拉曼光譜儀(Raman Spectroscopy，Raman) 25
2.3.8 比表面積與孔隙度分析儀(Specific Surface Area and Porosimetry Analyzer，BET) 27
第三章 三維結構(3D)多孔相石墨烯包覆黃銅礦(CuFeS2)的奈米複合材料作為檢測蔬菜中農業危害（甲基對氧磷）的新興電催化劑 28
3.1 前言 28
3.2 實驗步驟 30
3.2.1 材料和設備 30
3.2.2 材料GOS和 GOS@CuFeS2合成方式 30
3.2.3 CuFeS2奈米材料製造 30
3.2.4 GOS@CuFeS2薄膜在網版印刷碳電極上的修飾製備 31
3.3 結果與討論 31
3.3.1 GOS@CuFeS2奈米複合材料表面結構分析 31
3.3.2 MOX的電催化特性 34
3.3.3 pH值的影響 36
3.3.4 以微分脈衝伏安法DPV來測定MOX 36
3.3.5 以電極穩定性、可重複使用性和再現性研究 40
3.3.6 真實樣品分析 40
3.4 結論 42
第四章 一種新型高效能的B / N共摻雜中孔洞碳材料用於檢測異煙肼的電化學感測器 43
4.1 前言 43
4.2 實驗步驟 44
4.2.1 化學藥品和試劑 44
4.2.2 儀器 45
4.2.3 BNDC材料的合成以及修飾電極的製備 45
4.3 結果與討論 46
4.3.1 材料表面結構分析 46
4.3.2 電化學阻抗圖譜（EIS）和表面積研究 49
4.3.3 BNDC修飾電極對INZ的電催化效應 51
4.3.4 BNDC修飾電極對INZ的電流感測 54
4.3.5 BNDC修飾電極的選擇性、穩定性和再現性 55
4.3.6 BNDC/SPCE修飾電極的實用性 57
4.4 結論 57
第五章 開發以氧化鋁金屬奈米粒子為基底的電催化劑應用於檢測氫離子幫浦抑製劑(奧美拉唑)及儲能材料 58
5.1 前言 58
5.2 實驗步驟 59
5.2.1 化學材料和設備 59
5.2.2 Al2O3奈米材料的回收率 60
5.2.3 Al2O3奈米粒子改質GCE的製備 61
5.3 結果與討論 61
5.3.1 材料結構形態特性 61
5.3.2 修飾電極的阻抗圖譜和有效表面積測量 63
5.3.3 修飾電極對OMZ檢測的電化學響應 65
5.3.4 濃度和pH值的影響 67
5.3.5 掃描速率對Al2O3 NPs/GCE感測OMZ的影響 67
5.3.6 微分脈衝伏安法用於OMZ的定量檢測 68
5.3.7 修飾電極對OMZ的選擇性 69
5.3.8 感測器的再現性和耐用性 70
5.4 應用於超級電容器的電化學測量法 71
5.4.1 Al2O3奈米粒子的GCD測量 72
5.4.2 Al2O3奈米粒子的EIS研究 73
5.4.3 Al2O3奈米粒子的穩定性 74
5.5 結論 74
參考文獻 75

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