近年來，石墨烯量子點（GQD）作為新穎零維度的奈米材料備受關注，相較於現今應用之材料，其螢光反應及電化學特性具有更好的優勢及表現。GQD獨特性質包含小尺寸、高度生物相容性、光穩定性、強電活性和大比表面積，使其成為適合多種應用層面的最佳選擇。然而，應用GQD材料領域尚處於初發展階段，因此仍然充滿各種挑戰及可能性。利用GQD作為基底的奈米複合材料，由於其獨特的物理化學性質和優異的生物相容性，已於各種研究應用中成為首屈一指的焦點，特別是在能量儲存和生物醫學相關的領域。雖然目前許多奈米複合材料已透過高階技術進行改質優化，但是秉持簡單與成本低的途徑發展優異性能之能源裝置及生物感測器的奈米材料始終是一大挑戰。
本論文的重點是以GQD作為基底的奈米複合材料發展生物感測器和超級電容之應用。根據各應用的需求，石墨烯量子點表面的雜原子摻雜、官能基的修飾，以及將GQD與金屬氧化物如V2O5和HNT結合形成之奈米複合物，已經在本研究當中透過簡單的共價和電化學反應表現。透過電化學的特性可發現，對於其它組合相比，利用金屬氧化物為基底的奈米複合材料可以改進GQD的表現。
對於生物感測器的應用，摻氮石墨烯量子點（N-GQDs）與β-環糊精（β-CD @ N-GQDs）共價連接，並使用二茂鐵（FC）作為氧化還原指示劑，檢測線性濃度範圍在0.5 - 100μM之間，檢測限制為80 nM。另外，氮、硫共摻石墨烯量子點（N，S-GQDs）和金-聚苯胺（Au-PANI）陸陸續續被開發合成。在本研究中我們透過自組裝的方法製備以N，S-GQDs修飾的Au-PANI（N，S-GQDs @ Au-PANI）。這種新型奈米複合材料N，S-GQDs @ Au-PANI被用來製備用於檢測CEA的阻抗型免疫感測器，線性範圍為0.5〜1000 ng mL-1，檢測下限為0.01 ng mL-1。在另一項研究中，使用N-GQD（熒光探針）和V2O5奈米片(fluorescence nano-quencher and cysteine recognizer)在0.1 - 125μM的範圍內開發了半胱氨酸(cysteine)的熒光關閉檢測(fluorescence turn off-on detection)，檢測限為50 nM。所有開發用於測定膽固醇、CEA和cysteine的感測器都表現出高度選擇性，並且成功地應用於加標人血清樣品中，回收率極好。
除此之外，GQD @ HNT奈米複合材料具有30 - 50 W h kg-1和0.23 - 10.12 kW kg-1的優異能量與功率密度，並具有363 F g-1的高比電容。另外N-GQD @ Fe3O4-HNT的高比電容（418 F g-1）和良好的能量密度（42.1 - 58.1 W h kg-1）。而 N-GQDs @ HNT於電吸附效果優異的表現及施加電壓1.2V時電吸附電容和對鈉離子去除的高穩定性其，比電吸附容量（SEC）分別為20.05和mgg-1。
總結來說，本研究中所獲得的結果清楚地表明以GQD為基底的奈米複合材料，在作為用於生物醫學應用中的生物分子監測與診斷的潛在材料，並應用於製造優異性能的超級電容器設備和電容去離子化的材料，都有非常良好的結果。

Graphene quantum dots (GQDs) have recently emerged exponentially as a new class of zero-dimensional nanomaterial consisting fluorescent and electrochemical behaviour that show clear advantages over their currently existing counterparts. Their unique properties of small size, biocompatibility, photostability, electro-activity and large surface area make them suitable candidates for a plethora of applications. However, field of graphene quantum dots is still in a nascent stage and is filled with challenges and plenty of opportunities. GQDs based nanocomposites have gained great attention in multiple research applications, particularly in energy storage and biomedical fields due to their unique physicochemical properties and outstanding biocompatibility. Though, high end techniques have been applied in the fabrication of the nanocomposites, identification of simple and cost effective routes for development of nanomaterials with superior properties for energy devices and biosensors is always a challenge.
The present thesis is focused on development of GQDs based nanocomposites for their applications in biosensors and supercapacitors. Depending on the need for the application, hetero atom doping and/or functionalization of graphene quantum dot surface and combining GQDs with metal oxides like V2O5 and HNT for nanocomposite formation has been carried out by simple covalent and electrochemical reaction. The electrochemical characterizations show that improved performance could be achieved in case of metal oxide framework based nanocomposites compared to their individual components.
For the application of biosensor, nitrogen doped graphene quantum dots (N-GQDs) were covalently linked to β-cyclodextrin (β-CD@N-GQDs) and using ferrocene (FC) as redox indicator, a sensitive and selective electrochemical method for cholesterol detection in linear concentration range of 0.5 – 100 μM and the limit of detection is 80 nM has been developed. Further, nitrogen, sulphur co-doped graphene quantum dots (N, S-GQDs) and gold polyaniline (Au-PANI) were synthesized subsequently, for the preparation of N,S-GQDs decorated Au-PANI (N, S-GQDs@Au-PANI) via a self-assembly approach. This novel nanocomposite N,S-GQDs@Au-PANI was used to fabricate the impedimetric immunosensor for detection of CEA with wide linear range from 0.5 to 1000 ng mL-1 and low detection limit of 0.01 ng mL-1. In another study, fluorescence turn off-on detection of cysteine has been developed using N-GQDs (fluorescent probe) and vanadium pentoxide nanosheets (fluorescence nano-quencher and cysteine recognizer) in the wide range of 0.1 – 125 μM with a detection limit of 50 nM. All the developed sensors for determination of cholesterol, CEA and cysteine exhibited high selectivity and are successfully applied in spiked human serum samples with excellent recovery.
Additionally, GQDs@HNT nanocomposite delivered excellent energy and power densities of 30 - 50 W h kg-1 and 0.23 - 10.12 kW kg-1 with a high specific capacitance of 363 F g-1. In case of N-GQDs@Fe3O4-HNT high specific capacitance (418 F g-1) and an improved energy density (42.1 – 58.1 W h kg-1) was noted. N-GQDs@HNT show excellent electrosorption capacity and high stability toward sodium ion removal and the specific electrosorption capacity (SEC) 20.05 mg/g at 1.2 V in a 500 mg/L NaCl solution.
Overall, the obtained results clearly demonstrate the applicability of GQDs based nanocomposites as the potential material for bio-molecules monitoring and diagnosis in biomedical applications as well as superior electrochemical performance on supercapacitor devices and capacitive deionization.

Contents
Abstract………………………………………………………………………………........iii
摘要……………………………………………………………………………….…..…....v
Content……………………………………………………………………………………vii
List of figures……………………………………………………………………………..xii
List of tables……………………………………………………………………...……..xviii

Chapter 1 Introduction……………………………….....……………………………...…...1
1.1 Prelude …………………………………………………………………………….…...2
1.2 Graphene quantum dots………………………………………………………………...4
1.2.1 Properties …………………………………………………………………………4
1.2.2 Structure …………………………………………………………………………..5
1.2.3 Optical properties………………………………………………………………….5
1.2.4 Electrochemical properties…………………………………………………...……7
1.2.5 Biocompatability…………………………………………………………..………8
1.3 Synthesis methods………………………………………………………………...……8
1.3.1 Bottom up approach………………………………………………………….……8
1.3.2 Top down approach…………………………………………………………...…10
1.4 Changing PL and electrochemical properties by chemical modification………..……12
1.4.1 Heteroatom doping………………………………………………………………12
1.4.2 Controlling surface oxidation……………………………………………………13
1.4.3 Surface modification with small molecules………………………………...……14
1.5 Biosensor ……………………………………………………………………..………15
1.5.1. Classification of biosensor………………………………………………………18
1.5.1.1 Electrochemical biosensor…………………………………………...……19
1.5.1.2 Optical biosensors…………………………………………………………21
1.6 Supercapacitor…………………………………………………………………...……24
1.6.1 Classification of electrochemical capacitors………………………………..……26
1.6.2 Nanocomposites in Supercapacitor………………………………………………30
1.7 Capacitive deionization…………………………………………………………….…32
1.7.1 Water scarcity and the necessity for a promising treatment method……………32
1.7.2 Water treatment through electrochemical adsorption: Capacitive deionization (CDI)………………………………………………………………………………..…33
1.7.3 CDI technology developments……………………………………………...……36
1.7.4 Electrode material………………………………………………..………………37
1.7.5 Challenges of carbon-based materials in CDI……………………...……………39
1.8 Objectives……………………………………………………………………………..40
Chapter 2 Experimental section……………………………………………………………43
2.1 Materials………………………………………………………………………………44
2.2 Methodologies………………………………………………………………...………44
2.2.1 Synthesis of graphene quantum dots…………………………………….………44
2.2.2 Synthesis of N-doped graphene quantum dots………………………………..…45
2.2.3 Synthesis of N, S co-doped graphene quantum dots………………….…………46
2.2.4 Covalently bonded N-doped graphene quantum dots with β-cyclodextrin….. …46
2.2.4.1 Fabrication of β-CD@N-GQDs..................................................................46
2.2.5 N, S-GQDs decorated gold polyaniline nanowires………………………………46
2.2.5.1 Preparation of the Au-PANI………………………………………………46
2.2.5.2. Preparation of N, S-GQDs decorated Au-PANI…………………………47
2.2.6 Synthesis of N-Doped Graphene Quantum Dots-Decorated V2O5 Nanosheet….48
2.2.6.1 Exfoliation of bulk V2O5……………………………………………………………………...……48
2.2.6.2 Preparation of N-GQD@V2O5.................................................................................................... 49
2.2.7 Synthesis of graphene quantum dots coated halloysite nanotubes………....……49
2.2.7.1 APTES coating onto HNTs……………………………………….………49
2.2.7.2 Attachment of GQDs on APTES coated HNTs…………………...………49
2.2.8 Synthesis of N-doped graphene quantum dots anchored Fe3O4/halloysite nanotubes………………………………………………………………………………50
2.2.8.1 Synthesis of Fe3O4-HNT nanocomposites……………………………...…50
2.2.8.2 APTES coating on Fe3O4-HNTs……………………………………..……51
2.2.8.3 Attachment of N-GQDs on APTES coated Fe3O4-HNTs…………………51
2.3 Instruments used for characterization…………………………………………………52
2.3.1 Transmission electron microscope (TEM)……………………………….………52
2.3.2 Scanning electron microscopy (SEM)……………………………………...……52
2.3.3 Atomic force microscopy (AFM)…………………………………………..……52
2.3.4 X-Ray diffraction (XRD)…………………………………………………...……53
2.3.5 Raman spectroscopy…………………………………………………………..…53
2.3.6 Fourier Transform Infrared spectroscopy (FTIR)…………………………..……54
2.3.7 Thermo gravimetric analysis (TGA)………………………………………..……54
2.3.8 Surface area by Brunauer–Emmett–Teller (BET) analysis………………...……54
2.3.9 Fluorescence (FL)……………………………………………………………..…55
2.3.10 UV-Vis spectroscopy…………………………………………………………...55
2.3.11 X-ray photoelectron spectroscopy (XPS)………………………………………55
2.3.12 Electrochemical measurements…………………………………………………56
2.3.13 Capacitive deionization to sodium ion………………………………………….57
Chapter 3 Application of Graphene Quantum Dots Based Nanocomposites in Electrochemical Biosensor…………………..……………………………………………...58
3.1 Introduction…………………………………………………………………………...59
3.2 Cholesterol and CEA sensing methods……………………………………………….62
3. 2.1 Cholesterol sensing methods……………………………………………………62
3.2.1.1 Electrochemical sensing of cholesterol using β-CD@N-GQDs..................62
3.2.1.2 Analysis Cholesterol in human serum samples…………………………...64
3.2.2 CEA sensing methods……………………………………………………………64
3.2.2.1 Fabrication of the immunosensor…………………………………………64
3.2.2.2 Electrochemical measurements……………………………………………65
3.2.2.3 Analysis CEA in human serum samples…………………………………..65
3. 3 Results………………………………………………………………………………..66
3. 3.1 Characterization of the β-CD@N-GQDs nanosensing probe…………………...66
3.3.1.2 Stepwise characterization of the β-CD@N-GQDs sensor electrode using Cyclic Voltammetry……………………………………………………………….70
3.3.1.3 The effect of pH and time for the inclusion complexes formation between β-CD@N-GQDs nanoprobe and cholesterol……………………………………...72
3.3.1.4 Electrochemical detection of cholesterol using DPV……………………..73
3.3.1.5 Interference test……………………………………………………………76
3.3.1.6 Stability of β-CD@N-GQDs/FC.................................................................77
3.3.1.7 Detection of Cholesterol in serum samples……………………………….77
3.3.2.1 Characterization of N, S-GQDs@Au-PANI..............................................78
3.3.2.2 Stepwise characterization of the sensor electrode using Cyclic Voltammetry and impedance…………………………………………………………………….84
3.3.2.3 Electrochemical detection of CEA using EIS……………………………..86
3.3.2.4 Interference test and stability of the immunosensor……………………....92
3.3.2.5 Detection of Cholesterol in serum samples……………………………….93
3.4 Conclusions……………………………………………………………………94
Chapter 4 Application of N-doped Graphene Quantum Dots-Decorated V2O5 Nanosheet for Fluorescence Turn Off/On Detection of Cysteine……………………………………………96
4.1 Introduction…………………………………………………………………………...97
4. 2 Cysteine detection methods…………………………………………………………..99
4.2.1 Detection of Cysteine…………………………………………………………….99
4.2.2 Detection of cysteine in human serum samples………………………………...100
4.3 Results……………………………………………………………………………….100
4.3.1 Characterization of the N-GQDs……………………………………………….100
4.3.2 Characterization of V2O5 nanosheets and N-GQD@V2O5 nanocomposites…..102
4.3.3 Cysteine detection mechanism by N-GQD@V2O5..............................................105
4.3.4 Optimization and detection of cysteine by fluorescence……………………….108
4.3.5 Interference……………………………………………………………………..112
4.3.6 Detection of cysteine in human serum samples………………………………...112
4.4 Conclusions………………………………………………………………………….113
Chapter 5 Application of Graphene Quantum Dots Based Nanocomposites in Supercapacitor………………………………………………………………………………115
5.1 Introduction………………………………………………………………………….116
5.2 Results……………………………………………………………………………….118
5.2.1.2 Characterization of GQD-modified HNTs (GQD-HNTs)……………………118
5.2.1.3 Cyclic voltammetry analysis of GQD-HNTs…………………………………127
5.2.1.4 Charge – discharge studies of GQD-HNTs…………………………………..129
5.2.1.5 Electrochemical impedance analysis of GQD-HNTs………………………...130
5.2.1.6 Cyclic stability of GQD-HNTs……………………………………………….132
5.2.1.7 Ragone plot…………………………………………………………………...133
5.2.2.1 Characterization of N-GQDs………………………………………………....133
5.2.2.2 Morphology and structural charactaerization of N-GQD@Fe3O4.............................136
5.2.2.3 Cyclic voltammetry analysis of N-GQD@Fe3O4-HNTs..................................143
5.2.2.4 Charge–discharge studies of N-GQD@Fe3O4-HNTs.......................................144
5.2.2.5 Electrochemical impedance analysis of N-GQD@Fe3O4-HNTs......................146
5.2.2.6 Cyclic stability of N-GQD@Fe3O4-HNTs........................................................148
5.2.2.7 Ragone plot of N-GQD@Fe3O4-HNTs............................................................149
5.3 Conclusions………………………………………………………………………….150
Chapter 6 Nitrogen Doped Graphene Quantum Dots Coated Nanotubes as Electrode for Enhanced Capacitive Deionization…………………………………………………………152
 6.1 Introduction…………………………………………………………………………..153
6.2 Results………………………………………………………………………………..155
6.2.1 Characterization of N-GQDs@HNT...................................................................155
6.2.2 Electrochemical Performance…………………………………………………..158
6.3.3 CDI Performance……………………………………………………………….160
6.4. Conclusions…………………………………………………………………………163
Chapter 7 Conclusion and Future Perspective…………………………………………….164
7.1 Conclusions………………………………………………………………………….165
7.2 Future scope of the work…………………………………………………………….168
7.3 References…………………………………………………………………………...170
List of publications………………………………………………………………………...207

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