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研究生： 游文德
Darwin Kurniawan
論文名稱： 微電漿合成石墨烯量子點及環境與生醫應用
Microplasma Synthesis of Graphene Quantum Dots for Environmental and Biomedical Applications
指導教授： 江偉宏
Wei-Hung Chiang
口試委員: 江偉宏
Wei-Hung Chiang
邱昱誠
Yu-Cheng Chiu
蕭偉文
Wesley Hsiao
龔仲偉
Chung-Wei Kung
郭霽慶
Chi-Ching Kuo
Kostya (Ken) Ostrikov
Kostya (Ken) Ostrikov
學位類別： 博士
Doctor
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2022
畢業學年度： 110
語文別： 英文
論文頁數： 151
中文關鍵詞： 微電漿 、發射可調 、氮摻雜石墨烯量子點 、納米傳感器 、納米溫度計 、複合材料 、水淨化
外文關鍵詞： microplasmas, emission-tunable, nitrogen-doped graphene quantum dots, nanosensors, nanothermometers, composites, water purifications
相關次數： 點閱：299  下載：0 
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  •  上一筆

    • 具有可調控發射特性的氮摻雜石墨烯量子點 (NGQD) 是用於研究和應用的有用材料。然而，從生物質前體生產具有明確納米結構的 NGQD 的規模化和可持續生產仍然難以捉摸。此處，我們報告了在環境條件下使用大氣常壓微電漿輔助可調電子軌域NGQD合成及應用於生物分子、金屬離子、溫度和 pH 值的多功能感測。原位光學發射和紫外-可見吸收光譜測量表明，等離子體誘導的羥基自由基和溶劑化電子定義了 NGQD 的 N 摻雜劑構型和表面官能基，從而產生了發射可調的 NGQD。只在一小時內，單個微電漿可以產生穩定的膠體 NGQD 分散體，濃度為 100 μg/mL，可用至少 100 次 PL 感測，並且該過程具有可擴展性。
    有效和精確地感測癌症和神經遞質生物標誌物，包括葉酸 (FA)、多巴胺 (DA) 和腎上腺素 (EP)，對於癌症和神經系統疾病的早期檢測和診斷以及新藥的開發至關重要。通過調節 pH 值，FA 的選擇性感測範圍為 0.8 – 80 µM，DA 和 EP 的選擇性感測範圍為 0.4 – 100 µM，FA 的感測限 (LoD) 非常低，分別為 81.7、57.8 和 16.7 nM ，DA 和 EP，分別。發射可調的 NGQD 也可用作多功能納米傳感器，用於選擇性 Fe3+、Cu2+ 和 Hg2+ 感測，顯示出寬線性感測範圍 (0.5 – 300 µM) 和 47.9 nM 的 Hg2+ 低 LoD 和 10 – 80 °C 的靈敏溫度感測。
    另一方面，使用活性納米材料的 pH 傳感在從化學反應到生物化學、生物醫學和環境安全的許多領域，特別是在納米尺度上都有前景。然而，使用穩定、生物相容性和成本效益高的材料實現納米技術增強的快速、靈敏和定量 pH 感測仍然具有挑戰性。先進的光譜測量表明，官能調整的 NGQD 具有豐富的 -OH 官能團和隨著 pH 值的變化而穩定且大的斯托克斯位移，可以實現快速、無標記和離子穩定的 pH 傳感，傳感範圍從 pH 1.8 到13.6。 pH傳感的潛在機制與NGQD的-OH基團的質子化/去質子化有關，導致最大的pH依賴性發光峰位移以及電子軌域變寬或變窄。
    此外，我們研究的擴展涉及具有受控結構和性能的多功能金屬有機複合材料，這些複合材料對智能光電、藥物輸送、癌症治療、清潔能源和環境應用具有吸引力。在這裡，我們在環境條件下使用反應性非熱微電漿開發了具有均勻分散的 NGQD 和金納米粒子 (AuNP) 的輕質多孔金屬-石墨烯複合材料。 NGQDs 和 AuNPs 的協同作用加速了合成過程中的聚合物交聯，並確保了同時監測和淨化水的必要性能，包括用於重金屬離子PL感測，以及有機污染物的高吸附容量和快速催化降解。具有可調孔隙率和自愈能力的大面積複合材料可以通過快速且可擴展的電漿工藝製造，避免有毒化學品和高溫。該複合材料在 0.13 mM 4-硝基苯酚濃度下在 60 分鐘內實現 120 g g−1 水淨化，每天產生 2880 L kg−1 淡水。
    總體而言，我們的研究結果證明了具有可控光學特性的 NGQD 的微電漿納米工程的可能性，以及從可再生生物資源中可持續和可擴展地合成石墨烯納米材料的一步。我們研究的擴展工作為新興應用的高性能石墨烯-金屬複合材料的設計和生產提供了新的見解。

    Nitrogen-doped graphene quantum dots (NGQDs) with controlled emission properties are useful materials for fundamental research and applications. However, the scalable and sustainable production of NGQDs with defined nanostructures from biomass precursors remains elusive. Here we report a rational design of band structure engineering of colloidal NGQDs under ambient conditions using atmospheric-pressure microplasmas usable as the multifunctional nanosensors for biomolecules, metal ions, temperatures, and pH value. In situ optical emission and UV-Vis absorbance spectroscopy measurement reveals that the plasma-induced hydroxyl radicals and solvated electrons define the N-dopant configuration and surface functionalization of NGQDs, leading to emission-tunable NGQDs. In just one hour, a single microplasma jet can produce a stable colloidal NGQD dispersion with 100 μg/mL concentration lasting for at least 100 PL detections, and the process is scalable.
    The effective and precise detection of cancer and neurotransmitter biomarkers including folic acid (FA), dopamine (DA) and epinephrine (EP) are essential for early detection and diagnosis of cancer and neurological disorders and for the development of new drugs. By regulating the pH, the selective detection is achieved in broad ranges from 0.8 – 80 µM for FA and 0.4 – 100 µM for both DA and EP with the very low limits of detections (LoDs) of 81.7, 57.8, and 16.7 nM for FA, DA and EP, respectively. The emission-tunable NGQDs are also applicable as multifunctional nanosensors for selective Fe3+, Cu2+, and Hg2+ detection revealing broad linear detection range (0.5 – 300 µM) and low LoD of 47.9 nM for Hg2+ and sensitive temperature detection from 10 – 80 °C.
    On the other hand, pH sensing using active nanomaterials is promising in many fields ranging from chemical reactions to biochemistry, biomedicine, and environmental safety especially in nanoscale. However, it is still challenging to achieve nanotechnology-enhanced rapid, sensitive, and quantitative pH detection with stable, biocompatible and cost-effective materials. Advanced spectroscopy measurements reveal that functionality-tuned NGQDs with enriched –OH functional groups and stable and large Stokes shift along the variations of pH value can achieve rapid, label-free, and ionic-stable pH sensing with a wide sensing range from pH 1.8 to 13.6. The underlying mechanism of pH sensing is related to the protonation/deprotonation of –OH group of NGQDs, leading to the maximum pH-dependent luminescence peak shift along with the bandgap broadening or narrowing.
    Furthermore, the extension of our study involves multifunctional metal-organic composites with controlled structures and properties which are attractive for smart optoelectronic, drug delivery, cancer therapy, clean energy, and environmental applications. Here we develop lightweight, porous metal-graphene composites with uniformly dispersed NGQD and gold nanoparticles (AuNP) using reactive non-thermal microplasmas under ambient conditions. Synergy of NGQDs and AuNPs accelerates the polymer crosslinking during synthesis and ensures the requisite properties for simultaneous water monitoring and purification including reliable PL for heavy metal detection, as well as high adsorption capacity and fast catalytic degradation of organic pollutants. Large-area hierarchical composites with tunable porosity and self-healing ability can be fabricated by the fast and scalable plasma process avoiding toxic chemicals and high temperatures. The composite achieves 120 g g−1 water purification within 60 min at 0.13 mM 4-nitrophenol concentration and produces 2880 L kg−1 freshwater per day.
    Overall, our work demonstrates the possibility of the plasma-enabled nanoengineering of NGQDs with controlled optical properties and a step towards sustainable and scalable synthesis of graphene nanomaterials from renewable bioresources. The extension work of our study provides new insights into design and production of high-performance graphene-metal composites for emerging applications.

    Abstract i 摘要 iii Acknowledgement v Publications vi Table of Contents viii Abbreviations xii List of Figures xiii List of Tables xxiv Introduction xxvi Chapter I – Literature Review 1 I.1. Graphene Quantum Dots (GQDs) 1 I.1.1. Synthesis method 2 I.1.1.1. Top-down approach 3 I.1.1.2. Bottom-up approach 4 I.1.2. GQDs as PL-based nanosensors 6 I.1.2.1. PL-based sensing mechanisms 7 I.1.2.2. GQDs for biosensing 9 I.1.2.3. GQDs for heavy metal ion sensing 10 I.2. Microplasma 12 Chapter II – Experimental 14 II.1. Materials and Chemicals 14 II.2. Instrumentations 15 Chapter III – Microplasma-Enabled Colloidal Nitrogen-Doped Graphene Quantum Dots for Ultrasensitive and Selective Detection of Cancer and Neurotransmitter Biomarkers 17 III.1. Introduction 17 III.2. Experimental Section 20 III.2.1. NGQDs synthesis and purification 20 III.2.2. Biomarker selectivity test 21 III.2.3. Sensing of FA, DA, and EP 22 III.3. Results and Discussion 22 III.3.1. Effect of plasma discharge current and reaction time on NGQDs synthesis 22 III.3.2. Characterizations of NGQDs 24 III.3.3. PL-based biomarker sensing using NGQDs. 28 III.3.4. Control factors and sensing mechanisms. 37 III.4. Conclusions 45 Chapter IV – Microplasma-Nanoengineering of Emission Tunable Colloidal Nitrogen-Doped Graphene Quantum Dots as Smart Environmental-Responsive Nanosensors and Nanothermometers 46 IV.1. Introduction 46 IV.2. Experimental Section 50 IV.2.1. NGQDs synthesis and purification 50 IV.2.2. In situ study 50 IV.2.3. Metal ion sensing 51 IV.2.4. Temperature sensing 51 IV.3. Results and Discussion 51 IV.3.1. Microplasma synthesis of emission-tunable NGQDs 51 IV.3.2. TEM, XPS, and Raman characterizations of the synthesized NGQDs 54 IV.3.3. In situ OES and absorbance spectroscopy measurement of the plasma synthesis 60 IV.3.4. Selective metal ion sensing 65 IV.3.5. Temperature sensing 71 IV.4. Conclusions 73 Chapter V – Microplasma Band Structure Engineering in Graphene Quantum Dots for Sensitive and Wide-Range pH Sensing 75 V.1. Introduction 75 V.2. Experimental Section 78 V.2.1. Syntheses of NGQDs 78 V.2.2. Post-treatment process of the synthesized NGQDs 78 V.2.3. pH sensing 78 V.3. Results and Discussion 79 V.3.1. Synthesis and characterizations of NGQDs 79 V.3.2. Functionalization effect of NGQDs for pH sensing 90 V.3.3. pH sensing mechanism 96 V.4. Conclusions 98 Chapter VI – Plasma-Bioresource-Derived Multifunctional Porous NGQD/AuNP Nanocomposites for Water Monitoring and Purification 99 VI.1. Introduction 99 VI.2. Experimental Section 102 VI.2.1. Synthesis of NGQD/AuNP composites 102 VI.2.2. Purification of NGQDs 103 VI.2.3. Dye adsorption with NGQD/AuNP composites 103 VI.2.4. Catalytic degradation of 4-NP with NGQD/AuNP composites 104 VI.2.5. Metal ion detection using NGQD composites 104 VI.2.6. Metal ion detection using NGQD solution 104 VI.3. Results and Discussion 105 VI.3.1. Plasma synthesis of NGQD/AuNP composites 105 VI.3.2. Multifunctional water monitoring and purification of NGQD/AuNP composites 114 VI.3.3. Cr(VI) sensing with NGQD solution 120 VI.4. Conclusions 123 Chapter VII – Summary, Perspectives, and Future Works 125 VII.1. Summary 125 VII.2. Perspectives 125 VII.3. Future works 126 References 129

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