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研究生： 許立政
Li-Cheng Hsu
論文名稱： 氧化鋅奈米線陣列應用於表面增幅拉曼光譜分析
The Analysis of Surface-Enhanced Raman Spectroscopy based on Zinc Oxide Nanowire Arrays
指導教授： 陳良益
Liang-Yih Chen
口試委員: 陳景翔
none
劉豫川
none
陳貞夙
none
吳季珍
none
學位類別： 碩士
Master
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2012
畢業學年度： 101
語文別： 中文
論文頁數： 162
中文關鍵詞： 表面增幅拉曼光譜 、奈米球微影蝕刻 、氧化鋅奈米柱陣列
外文關鍵詞： surface enhanced Raman scattering, nanosphere lithography, zinc oxide nanorod arrays
相關次數： 點閱：597  下載：10 
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    • 本研究目的為藉著製備多維度結構基板，以應用於表面增幅拉曼光譜分析上。不同以往，早期表面增幅拉曼基板大多是將金屬奈米粒子製備於平面基板上，但本研究以傾斜-撈取法技術可簡易製備出規則排列的聚苯乙烯奈米球單層薄膜，間接製備出二氧化矽遮罩，以增加玻璃基板表面積及結構複雜性，且搭配著二氧化遮罩製備出有序的氧化鋅陣列來探討有序及無序的氧化鋅陣列於表面增幅拉曼訊號的表現。
    此外，在本研究中，選擇不同的還原劑製備出不同粒徑大小之銀奈米粒子，藉此被覆於先前所製備不同維度的基板上。從實驗中可得知：以硼氫化鈉做為還原劑可合成粒徑約20 nm的銀奈米粒子；以檸檬酸鈉做為還原劑則可合成出約為60 nm的銀奈米粒子。之後，將不同維度的基板先以聚乙烯吡啶中進行表面修飾，再將之含浸於銀奈米粒子溶液中。之後，使用Rhodamine 6G分子做為探測物質，進行比較各種不同維度基板之最佳化條件分析，最後並進行微量濃度之極限分析。在分析結果中可得知：以檸檬酸鈉為還原劑所合成之銀奈米粒子具有較大的粒徑，將其應用於不同維度的基板皆具有較強的拉曼增幅訊號；且在以氧化鋅奈米柱陣列的輔助之下，使基板結構由原先二維結構演進成三維結構，更進一步搭配奈米球微影蝕刻技術製備出有序氧化鋅陣列基板，可取得更強的拉曼增幅訊號。其增強因子計算出可增至6.61×107，並且可獲得1×10-13 M的Rhodamine 6G分子偵測濃度極限。

    In this study, the main tropic focused on the preparation of multi-dimensional nanostructure substrates for applying on the researches of surface enhanced Raman scattering (SERS). In the previous researches, the metal nanoparticles were prepared on the substrates directly for SERS. Herein, a simple dip-catch method was employed on assembling large area polystyrene spheres (PS)monolayer. By using the PS monolayer, an inverse opal structure could be made by filling in silicon dioxide sol-gel solution. In these two-dimensional nanostructures, the surface areas increased. In order to increase surface areas furthermore, the order zinc oxide nanorod arrays (ZnO-NRAs)were grown on glass substrate by using PS monolayer lithography method.
    In addition, different sizes of silver nanoparticles (Ag-NPs)were synthesized by using two different kinds of reduction reagent. When sodium borohydride was used, the sizes of Ag-NPs are around 20 nm； trisodium citrate dihydrate was used, the sizes of Ag-NPs are around 60 nm. Before decorating different sizes of Ag-NPs, the surfaces of multi-dimensional nanostructures substrates were modified by poly(2-vinylpyridine). In order to find the Ag-NPs decoration time, Rhodamine 6G (R6G)molecules was used as probe to determine the optimal conditions. Form analysis results, we could find SERS substrates decorated with large Ag-NPs have high Raman intensities, especially for ZnO-NRAs nanostructures were used as SERS substrates for auxiliary the original substrate structure from the original two-dimensional structure to three-dimensional structure, and ordered zinc oxide array substrate prepared with nanosphere lithography technology to gain a stronger Raman signal. The enhancement factor calculated about 6.61 ×107, and Rhodamine 6G molecular detection concentration limit of 1×10-13 M can be detected.

    中文摘要………………………………………………………………………………………………………………………………Ⅰ Abstract…………………………………………………………………………………………………………………………Ⅱ 致謝………………………………………………………………………………………………………………………………………Ⅳ 目錄………………………………………………………………………………………………………………………………………V 表目錄…………………………………………………………………………………………………………………………………Ⅹ 圖目錄………………………………………………………………………………………………………………………………ⅩI 第一章、 緒論…………………………………………………………………………………………………………………1 1-1 前言……………………………………………………………………………………………………………………………1 1-2 研究動機與目的………………………………………………………………………………………………………2 第二章、 理論基礎與文獻回顧……………………………………………………………………………………3 2-1 氧化鋅基本性質及成長方法…………………………………………………………………………………3 2-1-1 氧化鋅基本性質…………………………………………………………………………………………………3 2-1-2 氧化鋅製備方式…………………………………………………………………………………………………6 2-1-2-1 水熱法………………………………………………………………………………………………………………6 2-1-3 製備規則排列的氧化鋅奈米柱………………………………………………………………………11 2-1-3-1 奈米球微影蝕刻技術…………………………………………………………………………………12 2-2 金屬奈米粒子之製備方法……………………………………………………………………………………15 2-2-1 鹽類化學還原法…………………………………………………………………………………………………15 2-2-1-1 銀奈米粒子的製備………………………………………………………………………………………17 2-3 規則排列的微奈米結構…………………………………………………………………………………………19 2-3-1 微奈米結構的發現……………………………………………………………………………………………19 2-3-2 至備規則排列的微奈米結構……………………………………………………………………………20 2-3-3 自組裝……………………………………………………………………………………………………………………21 2-3-3-1 自然滴製法………………………………………………………………………………………………………22 2-3-3-2 旋轉塗佈法………………………………………………………………………………………………………25 2-3-3-3 Langmuir-Blodgett薄膜法……………………………………………………………………25 2-3-3-4 LB-like法………………………………………………………………………………………………………26 2-3-4 奈米球微影蝕刻……………………………………………………………………………………………………28 2-3-4-1 結構的分類………………………………………………………………………………………………………29 2-3-4-2 奈米球微影蝕刻的應用…………………………………………………………………………………31 2-4 拉曼散射原理及發展…………………………………………………………………………………………………39 2-4-1 拉曼散射發展歷史…………………………………………………………………………………………………39 2-4-2 固體中的晶格震盪…………………………………………………………………………………………………39 2-4-3 拉曼散射光譜原理………………………………………………………………………………………………42 2-5 表面增幅拉曼散射……………………………………………………………………………………………………45 2-5-1 表面增幅拉曼散射光譜的發現…………………………………………………………………………45 2-5-2 表面增強機制…………………………………………………………………………………………………………45 2-5-2-1 表面增強機制-電磁場增強效應……………………………………………………………………45 2-5-2-2 表面增強機制-化學增強效應…………………………………………………………………………47 2-5-3 表面增幅拉曼散射光譜相關計算方程式……………………………………………………………48 2-5-3-1 表面增幅拉曼強度計算……………………………………………………………………………………48 2-5-3-2 表面增幅拉曼散射增強因子計算……………………………………………………………………49 2-6 表面增幅拉曼發展…………………………………………………………………………………………………………53 2-6-1 表面增幅拉曼光譜的基板發展………………………………………………………………………………53 2-6-2 激發雷射光的選擇……………………………………………………………………………………………………62 第三章、 實驗步驟及方法…………………………………………………………………………………………………66 3-1 實驗流程簡圖…………………………………………………………………………………………………………………66 3-2 實驗要漂與設備儀器……………………………………………………………………………………………………67 3-2-1 藥品/耗材名稱…………………………………………………………………………………………………………67 3-2-2 實驗設備……………………………………………………………………………………………………………………71 3-2-3 分析儀器……………………………………………………………………………………………………………………73 3-3 實驗步驟…………………………………………………………………………………………………………………………79 3-3-1 清洗玻璃基板……………………………………………………………………………………………………………79 3-3-2 製備銀奈米粒子…………………………………………………………………………………………………………79 3-3-3 製備SERS基板-銀奈米粒子被覆於玻璃基板……………………………………………………81 3-3-4 製備SERS基板-銀奈米粒子被覆於二氧化矽遮罩基板……………………………………82 3-3-5 製備SERS基板-銀奈米粒子被覆於無序氧化鋅奈米柱陣列基板…………………86 3-3-6 製備SERS基板-銀奈米粒子被覆於有序氧化鋅規則陣列基板88 第四章、 結果與討論………………………………………………………………………………………………………………93 4-1以水熱法成長規則排列之氧化鋅奈米柱陣列…………………………………………………………………93 4-1-1製備聚苯乙烯奈米球單層薄膜………………………………………………………………………………………93 4-1-1-1技術一：以自然滴製法製備聚苯乙烯奈米球單層薄膜………………………………………93 4-1-1-2技術二：以傾斜-撈取法方式製備聚苯乙烯奈米球單層薄膜……………………………98 4-1-2製備具規排列及蜂窩狀結構之二氧化矽遮罩……………………………………………………………102 4-1-2-1以溶膠-凝膠法製備二氧化矽遮罩…………………………………………………………………………102 4-1-3以水熱法成長氧化鋅奈米柱陣列…………………………………………………………………………………107 4-1-3-1氧化鋅晶種層效應………………………………………………………………………………………………………107 4-2金屬銀奈米粒子製備與探討…………………………………………………………………………………………………119 4-2-1以檸檬酸鈉為還原劑來製備銀奈米粒子………………………………………………………………………119 4-2-2以硼氫化鈉為還原劑來製備銀奈米粒子………………………………………………………………………122 4-3不同維度及形態之SERS基板討論………………………………………………………………………………………124 4-3-1金屬銀奈米粒子之修飾時間……………………………………………………………………………………………127 4-3-2不同形態SERS基板……………………………………………………………………………………………………………141 4-3-3SERS基板之增強因子計算………………………………………………………………………………………………145 第五章、結論……………………………………………………………………………………………………………………………………155 第六章、參考文獻……………………………………………………………………………………………………………………………157

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