含氮超奈米晶鑽石膜在感測生物檢體應用上擁有極優異的靈敏度，本篇論文聚焦於利用含氮超奈米晶鑽石膜的成長機制研究，並探討其在各種生物感測器應用之設計。研究中建立了一高可靠度的含氮超奈米晶鑽石膜製程手法，此手法是建立於對其成長機制的深度了解，並藉此為基礎，分別將含氮超奈米晶鑽石膜應用於能檢測慢性阻塞性肺病之二氧化碳感測器設計，及開發可用於檢測高干擾性之低葡萄糖濃度範圍的唾液感測器，藉由以上研究之探討，進一步了解含氮超奈米晶鑽石膜在實際應用上之可行性。
在第一部分的研究中，主要針對含氮超奈米晶鑽石膜的成核成長方式進行深入探討研究。製程上，首先將矽基板浸泡在含有奈米鑽石及鈦顆粒的懸浮溶液中進行超音波聲震處理，藉由此方法在矽基板上產生出成核點後，接著利用微波電漿輔助化學汽相沉積法在特定分壓及能量條件下合成出含氮超奈米晶鑽石膜。在含氮超奈米晶鑽石膜之成核初期會形成一層氮化矽薄膜作為中間緩衝層，氮化矽薄膜中之氮原子在超奈米晶鑽石膜成核初期會擴散進入形成摻雜結構，以產生含氮超奈米晶鑽石膜。此外，將此薄膜進行圖案化製程後，其感測效能相較於平面結構來說，可以產生額外34%的訊號面積，顯示出含氮超奈米晶鑽石膜在生物檢體上之感測潛力。
在第二部分的研究中，將已成長完之含氮超奈米晶鑽石膜藉由化學浴共沉積法將氧化鋅成長於其上用於設計出檢測慢性阻塞性肺病之二氧化碳感測器。利用含氮超奈米晶鑽石膜多晶結構除了可以用作氧化鋅之成核點外，所提供成核點之位置亦可同時讓氧化鋅形成緻密且如花狀之形貌。研究中亦發現當氧化鋅成長於含氮超奈米晶鑽石膜上時，形成之薄膜性質會以類似兩半導體材料相接後所產生之異質接面結構呈現。結果顯示，本研究所開發之二氧化碳感測電極針對在4－15%的二氧化碳濃度區間擁有優秀的線性關係，其R2值高達0.9903，顯示其應用於感測二氧化碳之能力。
在最後一部分的研究中，沿用氧化鋅成長於含氮超奈米晶鑽石膜上之優異異質接面結構，再結合二茂鐵作為輔助訊號增強之中介體來製備成電極，以開發出可用於檢測高干擾性之低葡萄糖濃度範圍的唾液感測器。從研究結果顯示，電極在搭配液態葡萄糖氧化酶的條件下可以在20－600 μM的葡萄糖濃度區間展現出804.11 μA/mMcm2的優異靈敏度，且其R2 值為0.9926，而在含有干擾物的人工唾液測試條件下，於50－400 μM的葡萄糖濃度範圍中表現出高達1012.35 μA/mMcm2的靈敏度，其R2 值為 0.9912。此唾液葡萄糖感測電極所呈現之結果再次驗證了含氮超奈米晶鑽石膜在生物檢體感測上的應用潛力。

This dissertation explores the effective methods for developing high performance biosensors using nitrogen-incorporated ultrananocrystalline diamond (NUNCD) films. In this study, we focus on the growth evolution of NUNCD and discuss the design in various applications of biosensors. Herein, we can further understand the feasibility of the practical application of NUNCD films.
In the first part of the study, the nucleation and growth methods of NUNCD films are mainly discussed in-depth. In the process, the silicon substrate is first ultrasonicated in a suspension solution containing nano-diamond and titanium particles. Subsequently, NUNCD films were synthesized by microwave plasma enhanced chemical vapor deposition (MPECVD) under specific partial pressure and energy conditions. At the initial nucleation stage of the NUNCD films, a silicon nitride (Si3N4) film was formed as an intermediate buffer layer to provide the nitrogen doping in the UNCD films, creating the NUNCD films. In addition, the sensing performance of patterned NUNCD (P-NUNCD) films is higher than the pristine NUNCD films for dopamine (DA) detection. The sensing performance of P-NUNCD can generate an additional 34% signal area compared with the pristine NUNCD, indicating the potential of the NUNCD films on biological samples.
In the second part of the study, bidens-like zinc oxide (b-ZnO) was grown on the pristine NUNCD films by coprecipitation method, which was designed to detect chronic obstructive pulmonary disease (COPD). The NUNCD films act as nucleation sites for the growth of b-ZnO and induce a dense morphology with bidens-like structure. Additionally, the heterojunction structure of b-ZnO and NUNCD layers can improve the CO2 sensing performance, resulting in the purpose of COPD detection. The results show that the CO2 sensor developed in this study has an excellent linear relationship in the range of 4－15% CO2 concentration, and its R2 value is as high as 0.9903, which shows its ability to be used for CO2 detection.
In the final part, the extraordinary heterojunction structure of b-ZnO/NUNCD films was used as an easily oxidized layer. The ferrocene (FC) was then coated on the b-ZnO/NUNCD and performed as a mediator for auxiliary signal enhancement. Moreover, a liquid enzyme (glucose oxidase, GOx(l)) was introduced into the detection system, providing specificity. The results show that the salivary glucose sensors can exhibit an excellent sensitivity of 804.11 μA/mMcm2 in the glucose concentration range of 20－600 μM with the GOx(l), and its R2 value is 0.9926. The sensors also exhibit a high sensitivity with 1012.35 μA/mMcm2 in the 50－400 μM under artificial saliva and interferences, and its R2 value is 0.9912. The results presented by the salivary glucose sensing electrode once again verified the application potential of the NUNCD in the sensing of biological samples.

摘要 ii
Abstract iv
Acknowledgment vi
Table of contents vii
List of tables xii
List of figures xiii
Chapter 1. Overview 1
1.1 Introduction of biomarker for specific diseases 1
1.1.1 Parkinson's disease 1
1.1.2 Chronic obstructive pulmonary disease 3
1.1.3 Diabetes mellitus 5
1.2 Introduction of recently detecting methods for specific diseases 7
1.2.1 Parkinson's disease – Dopamine 7
1.2.2 Chronic obstructive pulmonary disease – CO2 9
1.2.3 Diabetes mellitus – Salivary glucose 13
1.3 Introduction of biosensor materials for specific diseases 17
1.3.1 Detection of dopamine 17
1.3.2 Detection of CO2 18
1.3.3 Detection of salivary glucose 20
1.3.4 Introduction of lab studies 21
1.3.5 Main purpose of this study 26
Chapter 2. Experiments and characterizations 29
2.1 Fabrication of electrode 29
2.1.1 Pretreatment of substrate 29
2.1.2 Synthesis of NUNCD film 29
2.1.3 Synthesis of b-ZnO film 30
2.1.4 Preparation of PEI-PEG layer 30
2.1.5 Synthesis of ferrocene nanoparticles 31
2.2 Characterization techniques 31
2.2.1 Raman spectroscopy 31
2.2.2 X-ray diffraction analysis 31
2.2.3 X-ray photoelectron spectroscopy 32
2.2.4 Fiels emission scanning electron microscopy 32
2.2.5 Spherical-aberration corrected field emission transmission electron microscope 32
2.2.6 Electrochemical workstation 33
Chapter 3. Nitrogen-Incorporated Acicular-Shaped Nanodiamond Films for Dopamine Detection 35
3.1 Research background 35
3.2 Results and discussion 37
3.2.1 Characterizations of bonding and crystallinity 37
3.2.3 Analyses of depth distribution by XPS 43
3.2.4 Characterization cross sectional view by STEM 46
3.2.5 Analyses of detection performance for dopamine sensing 48
3.2.6 The growth evolution of NUNCD films 51
3.2.7 Comparison of the present work with other reports on dopamine detection 54
3.3 Summary 55
Chapter 4. Human Exhalation CO2 Sensor Based on the PEI-PEG/b-ZnO/NUNCD/Si Heterojunction Electrode 56
4.1 Research background 56
4.2 Results and discussion 59
4.2.1 Characterizations of crystallinity by XRD pattern 59
4.2.2 Characterizations of the morphology and conductivity 60
4.2.3 Characterizations of cross sectional view by FESEM and STEM 64
4.2.4 Analyses of detection performance for CO2 sensing 67
4.2.5 Pathway of CO2 detection by PEI-PEG/b-ZnO/NUNCD/Si 72
4.2.6 Comparison of the present work with commercial products on COPD detection 75
4.3 Summary 76
Chapter 5. A Noninvasive Salivary Sensor Based on Ferrocene/b-ZnO/NUNCD/Si Heterojunction Nanostructures for Glucose Sensing in Neutral Condition 77
5.1 Research background 77
5.2 Results and discussion 80
5.2.1 Characterizations of crystallinity by XRD patterns 80
5.2.2 Characterization of the morphology by FESEM images 82
5.2.3 Characterization of the cross sectional view by TEM 85
5.2.4 Analyses of electrochemical performance for glucose sensing 87
5.2.5 Analyses of bonding and stability by XPS 97
5.2.6 Pathway of glucose detection by FC/b-ZnO/NUNCD/Si 100
5.2.7 Comparison of the present work with other reports on salivary glucose detection 101
5.3 Summary 102
Chapter 6. Conclusions 103
References 105
Publications and conference award 126

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