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

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姓名

秦佳寬(Jia-Kuan Qin) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

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
(Fabrication of Carbon Nanostructures with Size-Tunable Pores for Molecular Sensing through Surface Enhanced Raman Scattering)

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★ 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
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★ 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)

本研究我們開發了一種製備高質量多孔碳材料的方法，通過聚苯乙烯-b-4-乙烯基?啶（PS-b-P4VP）嵌段共聚物（BCP）作為碳源的薄膜直接熱解。在熱解之前，通過溶劑蒸氣退火（SVA）處理自組裝的BCP奈米區域，然後進行表面重建以獲得多孔模板。我們發現，可以通過使用不同的初始形態或表面重建的溫度來調整孔徑。得到的具有相當大比表面積的多孔膜，可作為表面增強拉曼光譜（SERS）的優良基材，用於物理吸附羅丹明6G的分子傳感。在奈米結構表面含有的豐富的氮原子在促進通過化學機制產生，在拉曼增強中起關鍵作用。最重要的是，我們觀察到銀奈米粒子的加入能讓聚苯乙烯-b-4-乙烯基?啶石墨化，且在燒結後能得到連續性的奈米結構。基於構建明確的網絡奈米結構的多孔模板的獨特結構為製造SERS基底提供了新的設計策略。

摘要(英)

We developed a method to fabricate porous carbon materials of high quality, via direct pyrolysis of poly(styrene-b-4-vinylpyridine) (PS-b-P4VP) block copolymer (BCP) as thin films as carbon resources. Prior to pyrolysis, self-asssembled BCP nanodomains were treated by solvent vapor annealing (SVA) followed by surface reconstruction to obtain the porous template. It can be found that the pore size can be adjusted by using different initial morphologies. The resultant porous films with a considerable specific surface area serve as an excellent substrate for surface-enhanced Raman spectroscopy (SERS), coupled with fluorescence quenching, for molecular sensing of physically adsorbed Rhodamine 6G. The abundant nitrogen atoms terminating on the surface of nanostructures play a critical role in promoting a large Raman enhancement generated via a chemical mechanism. Most importantly, the observed enhancement factors show a clear dependence on the mesoscale porosity within nanostructures, indicating that the chemical enhancement can be steadily tuned with control over the interfacial areas as a function of the initial morphology. And then, we observed that inlaid silver nanoparticles enabled the polystyrene-b-4-vinylpyridine to be graphitized and that a continuous nanostructure could be obtained after sintering. The unique architecture of the porous template based on the construction of a building block of a well-defined network nanostructure provides a new design strategy for fabricating SERS substrates.

關鍵字(中)

★ 嵌段共聚物
★ 孔洞材料
★ 薄膜
★ 拉曼光譜
★ 拉曼訊號增強

關鍵字(英)

論文目次

摘要...................................ii
Abstract...............................iii
致謝...................................iv
目錄...................................v
圖目錄.................................viii
表目錄.................................xiii
第一章序論...........................1
第二章簡介...........................3
2-1嵌段共聚物之自組裝行為..............3
2-1-1熱退火（Thermal annealing）.......7
2-1-2溶劑退火（Solvent annealing）.....8
2-2表面重建（Surface reconstruction）..11
2-3薄膜應用............................13
2-4拉曼光譜學..........................21
2-5表面拉曼光譜訊號增強原理............23
2-5-1化學增強型基材....................24
2-5-2電磁場增強型基材..................26
2-6實驗動機............................30
第三章實驗............................31
3-1高分子材料..........................31
3-2 溶劑藥品與基材.....................32
3-3 實驗儀器...........................33
3-4 試片製備與實驗步驟.................33
3-4-1矽晶基材(Si)清洗基材..............33
3-4-2矽晶基材(SiOx/Si)清洗基材.........33
3-4-3基材表面改質......................33
3-4-4 P(S-b-4VP)薄膜的製備.............34
3-4-5富含氮之碳膜的製備................35
3-4-6鑲嵌奈米粒子之基材的製備..........35
3-5 儀器分析...........................36
3-5-1原子力顯微鏡......................36
3-5-2光學顯微鏡........................37
3-5-3場發射掃描式電子顯微鏡............38
3-5-4 拉曼光譜儀.......................39
3-5-5 低掠角小角度X光散射訊號分析與擬合結構資訊....39
3-5-6 X射線光電子能譜儀................40
3-5-7高解析掃描穿透式電子顯微鏡........40
第四章結果與討論- 化學增強型基材......42
4-1透過微胞的聚變過程控制初始結構......42
4-1-1微胞聚變與裂變過程................42
4-1-2不同蒸氣壓下進行溶劑退火，對結構的影響........44
4-2藉由結構重組製備孔洞材..............47
4-2-1不同溶劑和不同分子量進行結構重建之探討........47
4-2-2重建結構溫度後對結構之影響........52
4-3孔洞碳膜製備及在拉曼增強訊號之表現..54
4-3-1重建結構後對碳膜之影響............54
4-3-2富含氮之孔洞型碳材在拉曼增強訊號上的效果......58
第五章結果與討論- 電磁場增強型基材....67
5-1鑲嵌銀奈米在富含氮之孔洞材..........67
5-1-1鑲嵌銀奈米在富含氮之孔洞碳材在拉曼增強訊號上的效果...67
5-1-2連續相固體銀基材..................73
第六章結論............................81
參考文獻...............................83

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指導教授

孫亞賢(Ya-Sen Sun)

審核日期

2018-7-19

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