各式奈米金屬結構已被大量探索，並用以製作高靈敏的表面增強拉曼基材，在食品安全、環境汙染、以及生物醫學的分析與檢測領域，佔有一席之地。然而，這些常見的方法通常需要繁瑣的製程、昂貴的設備，或是缺乏穩定的再現性。因此，本論文的研究目標即為開發具有量產潛力的表面拉曼增益基材，同時兼顧其高靈敏度以及高再現性的要求。
在本研究的第一部分，我們利用目前已經在太陽能產業廣泛使用的電極材料－奈米銀膠，作為提供電場增益的關鍵材料。首先，將商用奈米銀膠稀釋成不同濃度，接著將配製好的奈米銀膠溶液搭配旋轉塗佈法在4吋矽基板上沉積。隨著濃度的逐步下降，銀膠表面形貌將呈現三個階段的變化：少量的奈米裂紋、高密度奈米裂紋以及分散的奈米粒子陣列。接著，我們利用三維時域有限差分法(3D-finite-difference time-domain, 3D-FDTD)進行近場光學模擬，探索其電場增益的現象，並對亞甲基藍進行拉曼光譜量測。結果指出不同形貌的奈米銀膠結構展現出來的電場耦合增益與實際量測拉曼訊號趨勢高度相符，其中，高密度奈米裂紋展示出最佳的拉曼訊號。在此基礎上結合可攜式拉曼光譜儀(785 nm)，進行了後續實驗，其訊號增益幅度可達3.2×106，隨機取樣30次的重複性測試展現其優異的再現性(RSD =3.59%)。最終，我們測試不同領域10種常見有害性物質，並針對數種農藥進行混合分析以及在實際樣品(蘋果汁及蘋果皮)的檢測，展現其優異的靈敏度及實用性。
然而，有許多分析樣品本身或是所存在複雜環境，會在紫外光及可見光的雷射照射下產生強烈的螢光放射，從而造成大量的背景干擾。一旦發生螢光干擾，將會使得整個拉曼光譜失去其獨特的特徵峰，若使頻率較低的近紅外光(Near Infrared，NIR)雷射(如：785 nm或1064 nm)則可以有效降低螢光背景干擾。因此，在本研究的第二部分，我們將延伸第一部分之研究，針對近紅外光波段的雷射開發適合的表面增強拉曼散射基材。考慮到金奈米粒子較銀奈米粒子的表面電漿共振峰更靠近近紅外光波段，故選用奈米金膠。藉由對其表面形貌的調控，提升電場增益，並搭配近紅外光的可攜式拉曼光譜儀(785 nm 和1064 nm)，以此克服具有螢光干擾的拉曼待測物，提升光譜的可讀性，進而擴大實際臨床應用潛力。

Many different nanostructures have been explored to fabricate highly sensitive surface-enhanced Raman scattering (SERS) substrates for food safety monitoring, environmental pollution controlling, biomedical analysis and biosensing. However, the cumbersome fabrication processes, sophisticated equipment and low signal-reproducibility limited on-site detection of SERS. Thus, the aim of this thesis is to develop SERS substrates with ultrahigh sensitivity, high reproducibility and the potential of mass production.
In the first part, we design a simple, sensitive and scalable SERS substrate via breaking the conductivity of the commercial silver nanopastes (AgNPA). AgNPA, a widely explored electrode material in the photovoltaic industry, is a crucial material which could provide high electromagnetic (EM) field. By regulating the AgNPA concentration, the morphology of the spun-on AgNPA would transform from continuous film, dense nanocracks, to sparse nanoparticles. Then, the EM field distribution of AgNPA samples were evaluated via optical simulations and spectroscopic analyses. We surprisingly found that the EM intensity and electrical resistance gradually enlarged with decreasing AgNPA concentration. As the plentiful nanocracks were created, the AgNPA could generate the strongest EM intensity with large-area distribution, though its conductivity was broken. The optimal SERS substrate demonstrated a significant Raman enhancement factor up to 3.2×106, the detection limit of 10-9 M, and a signal reproducibility (RSD =3.59%) for methylene blue (MB), with a portable 785 nm Raman spectrometer. Moreover, to realize the wide applicability of the SERS substrate for on-site detection, 10 harmful substances in water and food were assessed. Finally, we demonstrated the great sensing performance in real samples by spiking thiram in apple juice and on apple peel. The limit of detection could reach 1 ppm and 3.91 ng/ cm2, respectively. The nanocrack-based SERS substrate fabricated via a simple, efficient and scalable fabrication process offer new opportunities for mass production and established high practical value for various applications.
However, with an excitation wavelength within UV-visible region, some of the organic compounds would occur naturally fluorescence which may cause high background signals and thus interfere spectral discrimination. Thus, in the second part, the similar strategy to the first part was extended by changing the plasmonic material to gold (Au). Also, portable Raman spectrometers with near infrared (NIR) laser (such as 785 nm or 1064 nm) were utilized to effectively reduce the fluorescence interference of analyte compounds or background. The commercial gold nanopaste (AuNPA) was selected because of the localized surface plasmon resonance peak of Au is typically closer to the NIR excitation wavelengths, as compared to Ag. The distribution of AuNPA could be well regulated through adjusting the concentration of AuNPA, soft-baking temperature and spin-coating rate, which would strongly influence the electric filed and the enhancement effect of Raman signal. We expect that the strategy can efficiently inhibit the fluorescence interferences, promoting the readability of Raman spectra, especially in future clinical applications.

致謝 I
摘要 II
Abstract IV
Table of contents VI
List of Figures IX
List of Tables XV
Chapter 1 Introduction 1
1.1 Motivation 1
1.2 Thesis Structure 2
Chapter 2 Literature Review 3
2.1 Surface-Enhanced Raman Scattering, SERS 3
2.1.1 Raman Scattering 3
2.1.2 Localized Surface Plasmon Resonance, LSPR 4
2.1.3 Surface-Enhanced Raman Scattering, SERS 9
2.1.4 Single Molecule Detection 12
2.2 Metallic Nanoparticles 13
2.2.1 Conventional Metallic Components—Gold and Silver 13
2.2.2 Ag Paste 14
2.3 Near infrared active SERS substrate 15
2.3.1 Fluorescence interference in Raman spectra 15
2.3.2 SERS detection with NIR excitation 18
2.4 The risks of the harmful chemical substances 21
Chapter 3 Wafer-scale nanocracks prepared from Ag nanopaste 23
3.1 The Design of Research 23
3.2 Experimental Section 25
3.2.1 Materials 25
3.2.2 Characterization 25
3.2.3 Fabrication of spun-on AgNPA/Si 25
3.2.4 Raman spectral measurement 26
3.2.5 FDTD simulations 26
3.2.6 Preparation of standard samples 26
3.2.7 Pesticide residues in apple juice and apple peel 27
3.3 Result and Discussion 28
3.3.1 Characterization of spin-coated Ag NCK arrays 29
3.3.2 Optical optimization of Ag NCK array for ultrasensitive SERS 33
3.3.3 Ultrahigh sensitivity of the Ag NCK SERS substrate: single molecule detection 36
3.3.4 Portable SERS measurement for on-site detection with Ag NCK array 39
3.4 Conclusion 52
Chapter 4 Nanocracks prepared from Au nanopaste for NIR SERS analysis 54
4.1 The Design of Research 54
4.2 Experimental Sections 55
4.2.1 Material 55
4.2.2 Characterization 55
4.2.3 Fabrication of spun-on Au-Si SERS Substrate 55
4.3 Result and Discussion 56
4.3.1 Solvent selection for Au nanopaste 56
4.3.2 Optimization of diluted ratio of AuNPA 58
4.3.3 Optimization of spin-coating rate and soft-baking temperature for AuNPA SERS substrate 60
4.3.4 The optimization of AuNPA substrate with 1064 nm portable Raman spectrometer 67
4.3.5 Particle size and gap effect on electric field enhancement 74
Chapter 5 Conclusion 81
5.1 Summary of Work 81
5.2 Future Work and Prospects 82
Reference 83

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