臺灣博碩士論文加值系統

奈米材料在環境和生物感測領域具有相當廣泛的應用潛力，螢光石墨烯量子點與金屬奈米顆粒均為常被應用於感測器領域的奈米材料。石墨烯量子點具有優異的光學與電化學特性，當摻雜異質元素時更可增加石墨烯量子點的螢光產率，而與金奈米顆粒結合時，更可提供催化能力來還原硝基酚類化合物，使得摻雜石墨烯量子點成為眾多奈米材料中，新穎且具多功能用途之潛力材料之一。
本研究的主要目的為開發新穎的氮,硫-共摻雜石墨烯量子點(N, S-GQDs)，除進行環境污染物(4-硝基苯酚和汞離子)的光學與生物標誌物(3-硝基-L-酪氨酸)的電化學檢測分析技術的開發與應用外，也藉由硫元素與金離子間的優異結合力，配合石墨烯量子點的還原能力，進行一鍋式合成Au@S-GQD複合材料，並應用作為4-硝基酚的分析檢測元件。研究發現GQD的顆粒粒徑為 XX – XX nm間，表面特性鑑定確定N及S摻雜在GQD晶格，在330 nm紫外光照射下，摻雜GQD在波長450 nm處具備最佳的螢光發射帶。在氮與硫共摻雜的情況下，石墨烯量子點的光學與電化學特性均能內顯著提昇，其中氮原子的摻雜，使量子產率增加到41.9％，而硫原子的引入則可強化配位相互作用，增加感測的靈敏度與選擇性。研究中發現4-硝基酚可藉由與S-GQD的 – 相互作用，造成石墨烯量子點的螢光猝滅，同時在10 nM – 200μM的範圍內具備相當優異的線性關係，其方法偵測極限在純水中0.7 nM，在受污湖水中則為3.5 nM。而汞離子在氮, 硫共摻雜石墨烯量子點存在環境中，具有相當優異的感測靈敏度與選擇性，其在純水中的線性範圍可達4個層級，方法偵測極限則可低至0.14 nM，另在實際染料廢水中的線性範圍也可達0.1 – 15 M間，回收率則介於96 – 116%間。另研究中也製備摻雜石墨烯量子點的紙製品感測器，在1分鐘內可快速篩選廢水中的4-硝基酚及汞離子，充分顯示摻雜石墨烯量子點優異的光學檢測能力。
研究中也製備金-硫間間優異的錯合能力與碳材的還原能力，製備金奈米＠的S-GQDs複合材料，結果明顯地指出S-GQDs可以還原金離子使其變成金奈米顆粒複合物。當中特別的是，在較長的碳骨架鏈中，結構中的硫原子可以縮短金離子還原成金納米複合材料的時間，因此只要簡單地調整金離子溶液之前驅物濃度，即可製備不同粒徑大小的 Au＠S-GQD。當Au離子濃度從50增加至150 μM時，Au @ S-GQD的平均直徑會從5nm增加到17nm平均粒徑。所製備的Au @ S-GQD顯現出優異的紫外-可見光吸收性能，對4-硝基苯酚的靈敏度可達4個數量級的範圍，在純水中的方法偵測測限為3.5nM，在諸多芳香族化合物共存環境中，仍具備相當優異的選擇性。此外，所開發的Au @ S-GQD感測平台也可成功應用於高污染食品廢水4-硝基苯酚的檢測分析，其線性範圍與方法偵測極限分別為0.05 - 50 μM及8.4 nM。
除光學檢測外，所開發的Au@S-GQD複合材料也具有相當優異的電化學特性，在5 – 200 mV/s的掃瞄速度下，Au@S-GQD在pH 7.4的水溶液環境中，展現優異的循環伏安特性，加上Au奈米顆粒及GQD sp2結構的優異導電性，讓Au@S-GQD具備相當低的電阻，因此可快速傳遞電子。當將Au@S-GQD批覆於濾紙形成紙製感測技術後，此感測器對3-硝基L-酪氨酸的感測線性範圍可高達8個數量層級(2  10-11 – 2  10-3 M)，方法偵測極限可低至18 pM，充分顯示Au@S-GQD紙製感測器在生物醫學的分析檢測的應用性。
此研究結果清楚顯示，利用N, S-共摻雜石墨烯量子點可快速進行不同分析物的檢測分析，而此研究也是國際上首次在不使用任何還原劑和加熱溫度情況下，利用S-GQD的還原能力，即可透過一鍋式反應製備Au＠S-GQD複合材料，且簡單藉由金奈米顆粒前趨物質濃度的調整，即可改變複合材料的尺寸與形貌。同時可利用Au@S-GQD進行環境與生物醫學的光學與電化學檢測應用。研究顯示本研究所開發的摻雜石墨烯量子點不僅具備獨特的光學與電化學特性，且具備相當優異的改質能力，能成功開發作為感測器檢測平台，進行環境與生物醫學不同目的的快速檢測分析技術開發。

Nanoscale materials have attracted potentials to impact the broad fields of heavy metal and biological sensing. In addition, the incorporation of nanomaterials and nanostructures into sensors leads to improve performance of detection capability. Fluorescent graphene quantum dots (GQDs) and metal nanoparticles are one of member nanomaterials have evoked significant attention in sensor. Many efforts have been made during recent years to develop portable sensors for environmental monitoring heavy metals. GQDs along doping with hetero structure specially sulfur (S) promise the advantageous physical and chemical properties of GQDs. The unique architecture of sulfur doped graphene quantum dots (S-GQDs) and the outstanding sensing performance provide a powerful impetus to use S-GQDs as a promising material for sensing.
Keeping all this in view, this thesis focused on developing novel S-GQDs via bottom up with their characterizations can offer further performance not only sensing but also as reducing agent. Current research includes: First of all, S-GQDs was fabricated using different doping agent as mercaptopropionic acid (MPA), mercaptosuccinic acid (MSA) and thiourea. Then, the optical methods were used to detect pollutant in environment as 4-nitrophenol (4NP) and mercury ion (Hg2+). The S-GQDs show the strong emission band at 450 nm under the irradiation of 330-nm UV light. 4-NP can serve as the fluoresce quencher by the  –  interaction with S-GQD, resulting in the linear decrease in fluorescence intensity after adding various concentrations of 4-NP in the range from 10 nM to 200 µM. As expected, The S-GQDs as the exhibitor shows the high analytical performance on 4-NP detection with limit of detection value of 0.7 nM in deionized water and 3.5 nM in lake water is obtained. Furthermore, S-GQDs based paper strip can rapidly screen 4-NP in wastewater within 1 min. We also investigate the reducing potential of S-GQDs for the fabrication gold nanocomposite. The results obtained in this thesis clearly demonstrate that S-GQDs can reduce Au ions to gold nanocomposite. The particle size of Au@S-GQD is tunable by simply adjusting the Au precursor concentration and the mean diameter increases from 5 to 17 nm when the Au precursor concentration increases from 50 to 150 µM HAuCl4. The Au@S-GQD exhibits good UV-visible absorption property, which is used for the sensitive detection of nanomolar level of 4-nitrophenol. A wide dynamic range of 4 orders of magnitude with the limit of detection (LOD) of 3.5 nM in deionized water is achieved. The UV-visible response of Au@S-GQD also shows good selectivity toward 4-nitrophenol detection over other aromatic and nitroarene compounds. In addition, the Au@S-GQD sensing platform is successfully applied to the detection of 0.05 – 50 µM 4-nitrophenol in highly contaminated food wastewater with LOD of 8.4 nM. Moreover, the N, S-codoped graphene quantum dots (N, S-GQDs) with high quantum yield were also fabricated by one-pot hydrothermal methods for highly sensitive and selective detection of nanomolar level of mercury ions (Hg2+) in water and wastewater. The as-prepared N, S-GQDs are uniform in size with mean particle size of 3.5  0.5 nm. The doping of nitrogen atom increases the quantum yield to 41.9%, while the introduction of S atoms enhances the selectivity of Hg2+ via strong coordination interaction. The fluorescence intensity of N, S-GQDs is quenched proportionally after adding Hg2+ concentrations and a dynamic range of 4 orders of magnitude with limit of detection of 0.14 nM is obtained in deionized water. The N, S-GQDs nanosensing probes can be successfully applied to the sewage and dye wastewater samples and a linear range of 0.1 – 15 µM with recovery of 96 – 116% is obtained. In addition, the coating of N, S-GQDs onto paper strip provides an excellently rapid screening and highly selective technique for Hg2+ detection in real wastewater.
Interestingly, the S-GQDs using mercaptosuccinic acid as sulfur source shows better as reduction agent comparing with N,S-GQDs. To the best our knowledge, there are the first time to use S-GQDs without adding any reduction agent and ambient temperature can synthesize gold nanocomposite via one simple step of mixing. In turn, the icosahedron shaped Au@S-GQDs were fabricated using S-GQDs as the linker and reductant. Electrochemical technique was used for sensing analysis 3-nitro L-tyrosine in human serum. There are no researches to fabricate different S-GQDs by using bottom up method for sensing analysis. Particularly, our research opens new strategy of S-GQDs as reducing agent to synthesize gold nanocomposite at room temperature in short time.
To the best our knowledge, our work is the first work have successfully fabricated different S-GQDs based on different sulphur sources via bottom up method. We have experimentally demonstrated S-GQDs by using pyrolysis and hydrothermal methods can fabricate different S-GQDs. Sulphur containing in graphene network shows not only good optical properties but also as reducing and capping agent to synthesize different size and shape of gold nanocomposites. On the other hand, our works also indicate that fabricated S-GQDs from different sources may have different applications. In particular, S-GQDs by using pyrolysis show excellent properties to control size and shape of gold nanocomposite. We propose the reason may come from the crystallization and surface-functionalized of GQDs. Our works demonstrate the reductant property of S-GQDs to synthesize gold nanocomposite via one simple mixing step at room temperature without adding any reductant. Our research results suggest a simple route to control different size and shape of gold nanocomposites. These results can be useful for synthesis gold nanocomposites or other metal nanocomposites and different applications.

Outline
中文摘要 I
ABSTRACT IV
ACKNOWLEDGMENTS VIII
Outline IX
LIST OF FIGURES XIV
LIST OF TABLES XXI
NOMENCLATURE XXIII
Chapter 1 1
Introduction 1
1.1 Motivation 1
1.2 Heavy metals and nitro-aromatic pollutant in environment 4
1.3 Biomarkers 6
1.4 Graphene quantum dots 8
1.4.1 Structure property 8
1.4.2 Fabrication 12
1.4.3 Doped GQDs 15
1.5 Gold nanoparticles 24
1.5.1 Structure property 24
1.5.2 Fabrication and applications 26
1.6 GQDs-based gold nanocomposite and application 31
1.7 Sensing technology for nanomaterial application 34
1.7.1 Fluorescence sensors 34
1.7.2 Colorimetric sensors 37
1.7.3 Electrochemical sensors 38
1.8 Objectives of this study 40
1.9 Content of this thesis 41
Reference chapter 1 43
Chapter 2 61
Sulfur doped graphene quantum dots as a fluorescence sensing probe for highly sensitive and selective detection of 4-nitrophenol in water and wastewater 61
Summary 62
2. 1 Introduction 63
2.2 Experimental section 65
2.2.1 Synthesis of S-GQDs 65
2.2.2 Characterization 66
2.2.3 Detection of 4-NP by S-GQDs 66
2.2.4 Determination of 4-NP in water and wastewater samples using S-GQDs 67
2.2.5 Fabrication S-GQDs-based paper test 68
2.3 Results and discussion 68
2.3.1 The structural characterization of S-GQDs 68
2.3.2 Detection of 4-NP by S-GQDs 74
2.3.3 Detection of 4-NP in real samples 83
2.3.4 Rapid screening of 4-NP using S-GQD-based paper strip 84
2.4 Conclusions 86
References chapter 2 89
Chapter 3 95
One-Step Synthesis of Size-Tunable Gold@Sulfur- Doped Graphene Quantum Dot Nanocomposites for Highly Selective and Sensitive Detection of Nanomolar 4-Nitrophenol in Aqueous Solutions with Complex Matrix 95
Summary 96
3.1 Introduction 97
3.2 Experimental 100
3.2.1 Synthesis of sulfur-doped graphene quantum dot (S-GQD). 100
3.2.2 Preparation of Au@S-GQD nanocomposites. 100
3.2.3 Surface characterization 100
3.2.4 Detection of 4-nitrophenol by Au@S-GQD nanocomposites. 101
3.2.5 Detection of 4-nitrophenol in real wastewater samples. 101
3.3 Results and discussion 102
3.3.1 Characterization of S-GQD and Au@S-GQD 102
3.3.2 Detection of 4-nitrophenol using Au@S-GQD 115
3.3.3 Detection of 4-nitrophenol in wastewater with complex matrix 123
3.4 Conclusions 127
Reference chapter 3 129
Chapter 4 134
Highly sensitive and selective detection of mercury ions using N, S-codoped graphene quantum dots and its paper strip based sensing application in wastewater 134
Summary 135
4.1 Introduction 136
4.2 Experimental 138
4.2.1 Synthesis of N, S-GQDs 138
4.2.2 Surface characterization 139
4.2.3 Detection of Hg2+ by N, S-GQDs 139
4.2.4 Detection of Hg2+ ions in real wastewater samples 140
4.2.5 Preparation of N, S-GQD-based paper strips for real wastewater detection 140
4.3 Results and discussion 141
4.3.1 Characterization of N, S-GQDs 141
4.3.2 Detection of Hg2+ using N, S-GQDs 149
4.3.3 Real wastewater analysis 155
4.3.4 Rapid screening of Hg2+ by N, S-GQD based paper strips 159
4.4 Conclusions 161
References chapter 4 163
Chapter 5 170
Gold@ sulfur-graphene quantum dots nanoparticle based paper electrode for highly sensitive and selective detection of 3-nitro tyrosine in human serum 170
Summary 171
5. 1 Introduction 173
5.2 Experimental details 176
5.2.1 Synthesize Sulfur doped Graphene quantum dots (S-GQDs) 176
5.2.2 Preparation AuNPs using S-GQDs as reductant agent 176
5.2.3 Electrochemical procedure 176
5.2.4 Determine 3NT level in human serum 177
5.3 Surface characterization 177
5.4 Results and discussions 178
5.4.1 Evaluation of reduction potential of S-GQDs for Au@S-GQDs synthesis 178
5.4.2 Detection of 3NT using Au@S-GQDs 187
5.4.3 Detection of 3NT in human serum using Au@S-GQDs 191
5.5 Conclusions 194
References chapter 5 195
Chapter 6 203
Conclusion and future scope of the work 203
6.1 Conclusions 204
6.2 Future scope of the works 207

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