設計、製造與鑑定由自對準型奈米環陣列所建構之準三維奈米元件

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研究生：	何啟誌 Ho, Chi Chih
論文名稱：	設計、製造與鑑定由自對準型奈米環陣列所建構之準三維奈米元件 Design, Fabrication, and Characterization of Quasi Three-Dimensional Nanodevices Fabricated by Self-Aligned Nanoring Structure Array
指導教授：	曾繁根 Tseng, Fan Gang
口試委員:	張嘉升周家復徐文光陳智郭昌恕
學位類別：	博士 Doctor
系所名稱：	原子科學院 - 工程與系統科學系 Department of Engineering and System Science
論文出版年：	2017
畢業學年度：	105
語文別：	英文
論文頁數：	106
中文關鍵詞：	拉曼光譜、奈米球微影、奈米環、自組裝二維膠體、繞射、聚苯乙烯
外文關鍵詞：	SERS, nanosphere lithography, nanoring, self-assembled colloids, diffraction, polystyrene
相關次數：	點閱：2 下載：0
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近年來因為大量的奈米材料被合成與生產，創造出各式各樣的可能性並應用於奈米元件中增加效能，使得奈米科技得到迅速發展。過去的文獻多集中於利用薄膜技術加工後製造二維奈米元件，在本論文中我們使用新穎奈米蝕刻技術製造准三維元件系統。這個系統除了可以利用週期性的二維環境外，也可於向垂直方向進行元件構築，以利用更多空間充實元件效能。當材料被侷限在垂直的三維奈米空間時，因為尺度效應，其性質表現會相當不同於塊材或者薄膜。
本論文主要分成兩個主體:第一個部分為大面積二維膠體晶體製造與奈米球微影技術、第二部分為新穎的自對準型奈米環陣列應用於表面增強型拉曼散射。我們利用自組裝方式，以聚苯乙烯膠體為構築材料，於氣液介面組裝膠體小球，使其形成大面積緊密堆積陣列。這種製造方式的特徵為低成本並且有機會發展成為規模性生產。這篇論文中，我們除了仔細研究二維膠體晶體的形成機制與優化製造系統，也額外發展二維晶體繞射技術以利監控生產過程，穩定批次間生產並維持品質。有能力穩定得到高品質二維膠體晶體後，續利用奈米球微影技術製造週期性奈米陣列。
第二個主題聚焦在使用新穎的奈米球微影技術製造自對準型奈米環陣列。表面增強型拉曼散射是奈米光學應用的一環，通常需要高密的光學熱點以增加拉曼訊號的感測敏感度。這裡所製造的自對準型奈米環陣列，是將奈米柱置放於奈米孔洞中的新穎結構。此結構經過鍍金後，會形成垂直式的三層奈米結構:第一層為金的奈米洞網絡陣列、第二層為附著於奈米柱上的奈米盤、以及第三層鑲埋在洞中的底層奈米環。於時域有限差分法的模擬中顯示，這三層奈米結構會互相作用並且生產出高密度與高電場增幅的光學熱點。這種準三維結構的設計會優於一般傳統上僅於二維平面上設計熱點，感度可增幅10倍。另一方面，由於我們有自行生產奈米結構的能力，也因此能調整奈米結構各方向維度，使其電漿共振區能夠符合激發雷射的波長，進一步提升表面增強型拉曼散射效能。藉由實驗設計與軟體模擬，我們可證明自對準型奈米環陣列之表面增強型拉曼散射敏感度來自於高密度的光學熱點，以及其中較強的電場增幅。

In the past decades, nanotechnology has rapidly progressed because enormous possibilities have been unlocked to manipulate materials toward high performance devices. Most works have focused on miniaturizing devices on two-dimensional (2D) surface by thin film technology. In the presented thesis, we adapted a quasi-3D system to reclaim volume from the vertical space and create directive arrangement for materials on 2D surface. The properties of material resident in the nanospace were strongly governed by the vertical and nanoscaled architectures, making the systems dramatically different from their thin film and bulk homologue.
In the first part, I introduce a facile route to create crystalline colloidal monolayer (CCM) via air/water interfacial self-assembly, which intrigues researches and engineers by the wafer-scaled nanofabrication without high capital costs. Here, I carefully studied the 2D colloidal system and made efforts to build a diffractive system that can non-invasively monitor the self-assembly process, with nanoscale precision, for batch-to-batch stability. With the assistance of stable and superior self-assembled colloidal array, the desired periodic nanostructure was realized by nanosphere lithography.
The second part is the application of CCM derived nanostructured array, related to light management, I use self-aligned nanoring array to enhance the numbers of hot-spots in vertical direction. A high-density-hotpots substrate is highly desirable in practical uses of surface enhanced Raman spectroscope (SERS). Upon locating a nanopillar in each nanowell, a nanohole network, nanoring and nanodisc was formed after gold thin film deposition and producing more edges per unit cell compared to simple nanowell or nanohole structures. Finite-difference time-domain (FDTD) simulations and SERS measurements both confirm that the magnitude of SERS signals can be enhanced compared to simple 2D design. In addition, the developed nanofabrication allowed people to fine tune the geometries of nanostructure, which affect the adsorption spectrum of the substrate. I purposely tune the resonance peaks to fit the incident laser wavelength for each substrate to their optimum condition and further confirmed the enhanced SERS sensitivity is from the enhanced numbers of hot-spots per unit cell.

Table of Contents
摘要
Abstract
誌謝
Chapter 1 Introduction……………………………………………………………1
Chapter 2 Fundamentals………………………………………………………….3
2.1 Nanostructured arrays……………………………………………………….3
2.2 Surface plasmons……………………………………………………………….4
2.3 Surface enhanced Raman scattering…………………………………….8
Chapter 3 Array-Typed Nanofabrication    …………………………………….11
3.1 Top-down pattering of nanoscaled mask…………………………….11
3.2 Bottom-up pattering of nanoscaled …………………………………….13
3.2.1Nanosphere lithography    …………………………………………………….14
3.2.2 Array of colloidal mask preparation………………………………….16
3.3 Etching technique………………………………………………………………21
3.3.1 Dry etching…………………………………………………………………….…21
3.3.2 Wet etching……………………………………………………………………….22
Chapter 4 Characterization………………………………………………………….25
4.1 Scanning electron microscopy (SEM) ………………………………….25
4.2 Atomic force microscope (AFM) ………………………………………….26
4.3 UV-Vis spectroscopy…………………………………………………………….27
4.4 Confocal Raman microscope……………………………………………….27
Chapter 5 Self-Assembly of Colloids at Interface…………………………29
5.1 Introduction…………………………………………………………………….……29
5.2 Experimental…………………………………………………………………………30
5.2.2 The production line………………………………………………………………30
5.2.3 The experimental line…………………………………………………………31
5.3.3 Materials and procedures…………………………………………………33
5.3 Result and discussion………………………………………………………………36
5.3.1 The formation of CCM[59] …………………………………………………36
5.3.2 Deposition of CCM onto a support………………………………………40
5.3.3 Monitoring of CCM via two-dimensional diffraction[63]………43
5.4 Conclusion    …………………………………………………………………….……59
Chapter 6 Self-Aligned Nanostructured Array for SERS Substrate    61
6.1 Introduction…………………………………………………………….……    61
6.2 Experimental…………………………………………………………………    64
6.2.1 Scheme of nanofabrication…………………………………………    64
6.2.2 Analytical enhancement factors………………………………….    69
6.3 Result and discussion………………………………………………………    73
6.4 Conclusion    …………………………………………………………………………86
Chapter 7 Summary & OUTLOOK………………………………………………87
7.1 Self-assembly of CCM………………………………………………………    87
7.1 SERS substrate……………………………………………………….…………    88
Reference……………………………………………………………..…………......……90
Appendix
Tables
Table 3-1 Summary of Top-down nanofabrication.………………………………………12
Table 3-2 Summary table of Bottom-up nanofabrication……………………………...…14
Table 3-3 The summary of etching technique for NSL……………...………...………… 24
Table 5-1 The time line of the evolution of self-assembly of CCM production………….35
Table 6-1 Summary of RIE etching parameters………………………………….……….69
Table 6-2 The abbreviations of the used parameters in AEF estimation……….………….71
Table 6-3 Summary of SERS performance. The Vgold is gold volume within the size of laser spot.……………………………………………………………………...………..……….85

Figures
Fig. 2-1 Plasmon excitation configurations: (a) SPP in Kretschman’s configuration, (b) BW-SPP in period dielectric configuration, and (c) LSP on nanoparticles………….......…..6
Fig. 2-2 Energy diagram of Rayleigh, Stokes Raman and anti-Stokes Raman scattering.………………………………………………………………………………..…..9
Fig. 3-1 Potential diagram as function of interparticle distance.(A) The position of primary and second energy minimum. The inset is OM image of the arrangement of colloids trapped at air/water interface. Where r is the interparticle separation and the V is the energy potential.………………………………………………………………………………..…..20
Fig. 3-2 Potential diagram as function of interparticle distance.(A) The position of primary and second energy minimum. The inset is OM image of the arrangement of colloids trapped at air/water interface. Where r is the interparticle separation and the V is the energy potential.………………………………………………………………………………..…..23
Fig. 5-1 The apparatus of production line. (a) Self-assembly system comprising syringe pump and L-B trough(b) Descuming system for removing surface contamination.  (c) Water replacement system driven by a peristaltic pump.................................................…..31
Fig. 5-2 The apparatus of production line. (a) Self-assembly system comprising diffractive kits. (b) Compression system operated by a computer controlled step motor.  (c) Upright OM and high speed camera supported by Prof. W.T. Juan and Prof. K.H. Lin in IoP, Academia Sinica……………………………………………..………………………..…..32
Fig. 5-3 Injection of PS colloids via a syringe pump. (B) Exerting shearing force to floating PS colloids for enhancing ordering. Ordering can be monitored by laser beam diffraction (C) transferring of 2D colloidal crystal onto substrate.………………..…………………..…..34
Fig. 5-4 Optical images, diffraction pattern and microscopic images of self-assembled PS colloids at air/water interface. The first row is the grating diffraction-resulted iridescence, which indicates the coverage of CCM. The result is further confirmed by laser diffraction in second row. In the third row, the arrangement of colloids is further confirmed by microscope.………………………………………….………………………………..…..39
Fig. 5-5 The CCM deposition on a silicon wafer (a) 1000 nm and (b) 220 nm PS array.………………………………………………………………………………..…..40
Fig. 5-6 Summary of common defects in CCM comprising vacancy, twinning, crack, boundary and size polydispersity.…………………………………………………..…..41
Fig. 5-7(a) SEM images of free-standing membrane of 220-nm-sized CCM/PEO hybrid on a punched stencil mask.  (b) Transfer of monolayers of 1000nmCCM/PEO hybrid onto the curved surface. The white scale bars are 5 μm.……………………………………..…..42
Fig. 5-8(A) Spatial arrangement of apparatus including L–B trough, laser beam and camera. (B) Illustration of the wave scattered by regularly-spaced PS colloids. (C) Arrangement of PS colloids on water surface.………………………………………………………..…..45
Fig. 5-9 The evolution of PS colloidal arrangement under isothermal compression. (A1) to (A4) are the photos of gradual compression of home-made L–B trough with PS colloids assembled at the air/water interface. The insets are laser diffraction patterns in each stage. (B1) to (B4) are the OM images of PS colloid arrangement that correspond to (A1) to (A4). Scale bars are 10 mm. The insets in panel (B) are the fast Fourier transform patterns.……………………………………………………………………………....…..48
Fig. 5-10(A) Triangular lattice of PS array. (B) Corresponding vectors in reciprocal space (C) and (D) 3-D sketch of Ewald sphere construction and reciprocal vectors.……………………………………………………………………………....…..50
Fig. 5-11(A) Closely-packed PS colloidal monolayer on an optically transparent glass. (B) Photos of apparatus and diffraction result, taken with a mobile camera and a monochrome camera, respectively. (C)Greyscale versus pixels numbers plotted according to the white broken lines drawn in inset of (B).……………………………………………..…....…..53
Fig. 5-12(A) The first- and second-order diffraction spots (B) The OM image captured at almost the same position as (A). (C) The analysis of the pair correlation function and Gaussian fitted curve (red).……………………………….……………………..…....…..55
Fig. 5-13(A) The evolution of diffraction spots varying with compression times. The first-, second- and third-order of diffraction spots, painted as red, green and blue, respectively, showing a radial escaping from the center spot. (B) The center-to-center distance d plotted as a function of compression time.…………………………………….…………......…..58
Fig. 6-16- 1 Fabrication procedures to produce three types of periodic arrays. (A) A starting array of PS colloids on a HSQ coated substrate. (B) Capping of a Cr layer on PS colloids and exposed HSQ surface as a mask. (A1) to (A2) are the fabrication procedures of a nanohole array. (B1) to (B3) presents the fabrication of HCL for obtaining a nanohole+disc array. By exchanging the step of (B2) to (B1), i.e. doing the CF4 RIE prior to the removal of PS colloids, the new sequence of (C1) to (C3) creates a nanoring cavity array. The scale bars in three SEM images are 600 nm.………………………….…………………....…..66
Fig. 6-2 Cross sectional SEM images of (A) Nanohole (B) Nanohole+disc (C) Nanoring cavity after gold deposition and lift-off masks. (D) Cross-sectional view of the formation of nanoring cavities…………………………………………………………………....…..67
Fig. 6-36- 2Geometric parameters of AEF measurement illustrated by cartoon.………70
Fig. 6-4(A) SEM image and AFM topography (inset) of a nanoring cavity array. The scale bar in the SEM image is 6 μm. (B) The open dots denote the line profiles of the cross sections corresponding to the white line in the inset of Fig. 2(A). The black solid line is the averaged profile fitted from several randomly-selected nanoring cavity unit cells. (C) A bird-eye-view SEM image of a nanoring cavity array. The scale bar is 600 nm…...…..74
Fig. 6-5 Comparison of measured and simulated reflectivity from (A) nanoring cavity (B) nanohole+disc (C) nanohole arrays with 55-nm-thick gold deposition and 500 nm period. The measured and simulated spectra were read according to left and right axis in each figure.………..……………………………………………………………………....…..76
Fig. 6-6(A) Stokes-shifted SERS spectra of R6G from the nanoring cavity arrays with different thickness of gold deposition. The intensity of aromatic C-C stretching at 1360 cm-1 is used for AEF calculation. (B) Comparison of the AEF from nanoring cavity, nanohole+disc, and nanohole templates with different thickness of gold deposition. The maximum AEF of 1.3x105 is observed from the nanoring cavity arrays when the thickness of gold deposition is 55 nm. The error bar is the standard deviation of measured SERS magnitudes from each set of measurements.………..…………………………………..78
Fig. 6-7Schematic diagrams (upper panels) and simulated field enhancement distributions (lower panels) of (A) a nanohole, (B) a nanohole+disc, and (C) a nanoring cavity unit cell in Z-X plane with thickness of gold equals to 55 nm. The colors of gold, dielectric HSQ, substrate and hot spots are presented as yellow, blue, green and red, respectively in schematic diagrams. The schematic hot spots are plotted mimicking the simulation results. The simulated field enhancement is displayed on a logarithmic scale. The E0 and K are amplitude of electric field and wave vector of incident light with λ = 633 nm. The dashed and solid lines are added to indicate the gold and HSQ boundaries………..…………………………………………………………………...80
Fig. 6-8 Cross sectional SEM images of nanoring cavity architecture (upper panels) and the corresponding field enhancement distribution by FDTD simulations (lower panels) with (A) thickness of gold deposition = 20 nm, (B) 55 nm, and (C) 80 nm in the Z-X plane. The connected and blunted boundary of gold layer is indicated by a gray dashed line in the SEM image of (C). All scale bars in SEM images are 200 nm.………..……………………82
Fig. 6-9(A) the reflectivity of nanohole and nanoring cavity with gold thickness of 200 nm and 55 nm, measured in water. (B) and (C) are the cross-sectional SEM images of nanoring cavity and nanohole corresponding to (A). The scale bar is 500nm. The dashed line in (A) signifies the laser wavelength of 633nm.………………………………………....…..84

                                

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