利用高分子模版製備具有表面增強拉曼訊號之奈米銀陣列基板

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施思羽(Szu-yu Shih) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

利用高分子模版製備具有表面增強拉曼訊號之奈米銀陣列基板
(Nanostructured Silver Arrays for SERS Fabricated within Block copolymer Nanotemplates)

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★ 製備具可調控孔洞大小的奈米結構碳材用於增強拉曼效應之研究	★ 結合嵌段共聚物自組裝及微乳化法製備三維侷限多層級結構
★ 嵌段共聚物/多巴胺混摻體自組裝製備三維多尺度孔隙模板	★ 弱分離嵌段共聚物與均聚物雙元混合物在薄膜中的相行為
★ 摻雜效應對聚(3,4-乙烯二氧噻吩):聚苯乙烯磺酸紫外光照-導電度刺激響應之影響與其應用	★ 可撓式聚(3,4-乙烯二氧噻吩):聚苯乙烯磺酸熱電裝置研究：微結構調控增進熱電性質
★ 由嵌段共聚物膠束模板化的多層級孔洞碳材：從膠束(微胞)組裝到電化學應用	★ 聚苯乙烯聚4-乙烯吡啶共聚物微胞薄膜之聚變與裂變動態結構演化之研究
★ 除潤現象誘導非對稱型團鏈共聚物薄膜之層級結構	★ 極性/非極性共溶劑退火法調控雙團鏈共聚物薄膜奈米微結構

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摘要(中)

論文的第一部分，利用調配不同濃度的聚苯乙烯聚2乙烯吡啶(Polystyrene-block-poly(2-vinylpyridine), P(S-b-2VP))溶液以控制高分子模板之表面覆蓋率，進而含浸至硝酸銀的乙醇溶液，藉由紫外光還原而得到點狀的有序銀粒子陣列。隨著紫外光曝曬的時間增加，高分子模板的劣化使得聚集的銀粒子無法受模版侷限，因而造成聚集的銀粒子散佈於基材上。藉由控制粒子間距以及觀察粒子隨著紫外光照射的變化可得知當銀粒子間距較小時，吸附上Rhodamine 6G後能夠有較強的表面增強拉曼效應。
本研究除了利用模板來控制粒子間距，在論文的第二部分使用聚苯乙烯聚４乙烯吡啶(Polystyrene-block-poly(4-vinylpyridine), P(S-b-4VP))經由溶劑退火的方式，製造圓球狀的微胞模版以及圓柱狀的微胞模版。形成圓球狀及圓柱狀的微胞模版含浸至乙醇，分別形成了具有奈米級孔洞的薄膜與指紋狀的奈米溝槽薄膜。進一步利用四種不同形狀的模板：圓球狀、圓柱狀、奈米孔洞與指紋狀的奈米溝槽，以氬氣電漿的方式還原銀離子得到不同形狀的奈米銀陣列。當增加氬氣電漿處理的時間，由圓球狀與圓柱狀模版所製成的奈米銀陣列較能維持模版給予的有序性。此外，當氬氣電漿處理三百秒後，藉由指紋狀的奈米溝槽模版製備的奈米銀陣列，吸附上Rhodamine 6G則具有較強的表面拉曼增強訊號。

摘要(英)

Tailor-made templates through self-assembly of block copolymers are capable of fabricating technologically nanostructured substrates. In this thesis, a sample but robust method is demonstrated to fabricate arrays of silver nanostructures with morphological diversity and a tunable adjacent gap for large area surface-enhanced Raman spectroscopy (SERS) substrates.
First, nanostructured silver arrays of adjustable particulate size and inter-particle distance were fabricated by block copolymer templates for SERS substrates. The templates were formed by polystyrene-block-poly(2-vinylpyridine), P(S-b-2VP), micelles. The silver arrays with various surface coverage were prepared by spin-coating from o-xylene solution of varied polymer concentration (0.3 and 0.8 wt%). Photochemical reduction was applied to reduce silver ions after the P(S-b-2VP) micellar films were immersed in ethanol containing AgNO3. The interplay between the reduction of Ag+ and the removal of the P(S-b-2VP) template during UV-exposure for various time intervals affect the growth and spatial order of Ag nanoparticles, which in turn influences their SERS properties.
Moreover, polystyrene-block-poly(4-vinylpyridine) was used to produce spherical micellar templates and cylindrical micellar templates through solvent annealing. Nanoporous and nanogrooves templates were made when spherical micellar templates and cylindrical micellar templates were immersed in ethanol. Spherical micelles, cylindrical micelles, nanoporous, and nanogrooves were utilized to fabricate silver arrays. Petal-like cluster, fingerprint clusters, network clusters and reverse fingerprint clusters were produced by reducing silver salts in BCP templates. Through long time of Ar plasma treatment, petal-like clusters and fingerprint clusters could maintain the order of spherical micellar templates and cylindrical micellar templates. Furthermore, reverse fingerprint clusters with R6G adsorption had the strongest SERS enhancement through Ar plasma treatment for 300 sec.

關鍵字(中)

★ 奈米銀
★ 拉曼

關鍵字(英)

★ silver nanostructured films
★ SERS

論文目次

摘要 i
Abstraction ii
Table of contents iv
List of figures vi
Chapter 1 Introduction 1
1.1 Micelle 5
1.1-1 Micellar thin films 6
1.1-2 Applications of micellar thin films 7
1.2 Surface chemical reductions 11
1.3 Surface Enhanced Raman Scattering 18
1.3-1 Fundamental theory 19
1.3-2 SERS substrate 22
1.4 Applications of SERS substrate 24
1.5 Motivation 29
Chapter 2 Experimental section 30
2.1 Materials 30
2.2 Instrument 30
2.3 Sample Preparation and Experimental 31
2.3.1 Substrate Cleaning 31
2.3-2 Surface modification 31
2.3-3 The preparation of di-block copolymer thin film 32
2.3-4 Production of metal nanoparticles 32
2.4 Instrumental Analysis 34
2.4-1 Atomic Force Microscope: 34
2.4-2 Field Emission Scanning Electron Microscope 35
2.4-3 Surface-enhanced Raman Spectroscopy 37
2.4-4 Grazing Incident Small Angle X-Ray Scattering 39
2.4-5 UV-vis spectrophotometer[70] 40
Chapter 3 Result and Discussion 42
3.1 Temporal evolution of growth of silver nanostructures by template-assisted photochemical reactions 42
3.1-1 Nanoparticles with a large gap distance 45
3.1-2 Nanoparticles with small gap distance 56
3.2 The evolution of growth of silver nanostructure within template-assisted through plasma treatment 64
3.2-1 The different between photochemical reaction and plasma treatment 65
3-2.2 The morphological evolution of silver nanostructured films with different templates 68
3-3 SERS of R6G absorbed on different silver nanostructures films fabricated through Ar plasma treatment 76
3-4 The growth of silver and the degradation of block copolymer through reduction process 80
Chapter 4 Conclusion 84
Chapter 5 Future Work 86
Reference 87

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指導教授

孫亞賢(Ya-Sen Sun)

審核日期

2012-7-3

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