三維有序金屬奈米管陣列應用於表面增強拉曼散射基材之研究

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研究生：	劉芝羽 Chih-Yu Liu
論文名稱：	三維有序金屬奈米管陣列應用於表面增強拉曼散射基材之研究 Metallic nanotube arrays as the surface-enhanced Raman scattering (SERS) substrate: Fabrication and properties
指導教授：	朱瑾 Jinn P. Chu
口試委員:	朱瑾 Jinn P. Chu 陳學禮 Hsuen-Li Chen 今榮東洋子 Toyoko Imae 江偉宏 Wei-Hung Chiang 盧凌 Ling Lu
學位類別：	碩士 Master
系所名稱：	工程學院 - 材料科學與工程系 Department of Materials Science and Engineering
論文出版年：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	122
中文關鍵詞：	貴重金屬、表面增強拉曼、金屬奈米管陣列、結晶紫、羅丹明 6G 、殼核結構
外文關鍵詞：	noble metal, SERS, metallic nanotube array, crystal violet, Rhodamine 6G, core-shell
相關次數：	點閱：322 下載：0
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表面增強拉曼散射光譜(Surface-enhanced Raman Scattering，SERS)因其可將原先拉曼光譜的訊號增強數倍，甚至可以偵測單一分子的訊號，使得SERS基板的相關研究在近年來受到重視。表面電漿子共振(Surface Plasmon Resonance, SPR)效應為SERS增強的重要決定條件，其受到材料、間距、尺寸及表面積等影響。本研究主題為探討不同SERS基材設計對於其拉曼增強效果的變化。透過半導體微影製程及物理氣相沈積技術，製造有序之金屬奈米管陣列，且其奈米管形狀、大小、間距皆可透過光罩設計進行調整。
本研究將分為三大部分，首先為透過2種常見合金及1種純金屬作為奈米管之材料，分別為鈦合金(Ti64)、7075鋁合金(AA)及純金，成功透過結構之參數調整，製備出直徑0.8 ?m、高度0.7 ?m的有序圓形金屬奈米管陣列。結合前人所製備的金屬奈米管陣列（718鎳合金、青銅、SS316不銹鋼、純銅和純銀），並利用結晶紫(crystal violet, CV)作為檢測SERS的待測物，發現純銀及純金之金屬奈米管陣列具有良好的SERS增強效果，其中又以純銀的效果最為顯著；其二，透過在圓形鋯基(Zr60Cu24Al11Ni5)金屬玻璃奈米管陣列（直徑為10 ?m、高度為0.7 ?m）上沈積金奈米顆粒，有效透過貴重金屬粒子及表面積的增加來增強拉曼增強效果，在利用CV及R6G為SERS待測物下，其最低偵測極限濃度(Limit of detection, LOD) 分別可達到10^-13 M及10^-9 M，增強因子分別為1.49x 10^8及8.41x 10^5，同時亦具有良好的再現性；最後，經由重新設計光罩，製備出三角形的金屬奈米管陣列，探討陣列材料、形狀、三角形外接圓直徑大小及偵測位置對於拉曼增強之影響，其中在不同材料選擇下，即使純銀單層金屬奈米管具有較好的拉曼增強，但其陣列的產率低，存在許多倒塌的奈米管，為求增加三角形奈米管陣列之產率，而後選擇將鎢基金屬玻璃(W50Ni25B25)鍍覆為中間層，第一層及第三層為純銀，形成三明治結構，支撐其奈米管結構。在利用R6G為SERS待測物下，其最低偵測極限濃度(Limit of detection, LOD) 可達到10^-10 M，增強因子為1.38 x 10^7，同時其相對標準偏差(RSD)為5.13%，成功製備三維的三角形金屬奈米管陣列，且具有可定點量測、有序規則之結構，及良好的拉曼增強效應，證實金屬奈米管陣列可有效的吸附待測分子應用於SERS檢測之相關應用。

Surface-enhanced Raman Scattering (SERS) can enhance the signal of the original Raman spectrum by several times and can even reach single-molecule detection. Therefore, the related research of SERS substrate has been paid more attention in recent years. Surface Plasmon Resonance (SPR) effect is an important determinant of SERS enhancement, which is affected by materials, spacing, size, and surface area. This study aims to explore the Raman enhancement effects of using different SERS substrate designs. By using the lithography process and physical vapor deposition technology, metallic nanotube arrays (MeNTAs) is then manufactured, and the shape, size, and spacing of the nanotubes can be adjusted through the mask design.
This research will be divided into three parts. Firstly, two common alloys and one pure metal are used as the material of nanotubes, namely titanium alloy (Ti64), 7075 aluminum alloy (AA), and pure gold. After the adjustment of deposition parameters, an ordered circular MeNTA with a diameter of 0.8 ?m and a height of 0.7 ?m was prepared. Combining the MeNTA (718 nickel alloy, bronze, SS316 stainless steel, pure copper, and pure silver) prepared by the predecessors, and using crystal violet (CV) as the SERS probe, pure silver, and pure gold MeNTAs was shown good SERS enhancement effect, and the effect of pure silver is the most significant. Secondly, by depositing gold nanoparticles on the circular Zr-based (Zr60Cu24Al11Ni5) metallic glass nanotube array (diameter 10 ?m, height 0.7 ?m) can effectively enhance the Raman enhancement effect owing to the properties of noble metal nanoparticles and the increment of surface area. Under the use of CV and R6G as SERS probe, the limit of detection of AuNPs@MeNTA can be reached 10^-13 M and 10^-9 M, respectively, the enhancement factors are 1.49x 10^8 and 8.41x 10^5, and it also shows good reproducibility. Finally, through the redesign of the mask, a triangular MeNTA is prepared, and the following study is to discuss the Raman effect of material, shape, diameter of triangular nanotube, and detection position. Among them, by discussing the Raman effect of different compositions, even if pure silver monolayer MeNTA has a better response to Raman enhancement, the yield of its array is low, indicating many nanotubes are collapsed. In order to increase the yield of the triangular MeNTA, W-based metallic glass (W50Ni25B25) is then selected as the buffer layer., and the first and third layers are made of pure silver to form a sandwich structure, which can support the structure of nanotubes. R6G was selected as the Raman probe for triangular W-TFMG@MeNTA, the limit of detection can reach as low as 10-10 M, the enhancement factor is 1.38 x 10^7, and its relative standard deviation (RSD) is 5.13%. The three-dimensional triangular MeNTAs provides a sensitive SERS substrate with a well-ordered structure, and also can reach fixed-point measurement, indicating that MeNTA can effectively adsorb the molecules to apply in SERS application.

摘要 ............................................................................................................................................... I Abstract.........................................................................................................................................II Acknowledgements .................................................................................................................... IV Content......................................................................................................................................... V List of Figures.............................................................................................................................IV List of Tables ............................................................................................................................... X Chapter 1 Introduction............................................................................................................... 1
1 Objectives of study ........................................................................................................ 2 Chapter 2 Literature Review ..................................................................................................... 3 2.1 Plasmonics ..................................................................................................................... 3 2.1.1 Surface plasmon resonance (SPR)...................................................................... 3 2.1.2 Localized surface plasmon resonance (LSPR) ................................................... 4 2.2 Raman spectroscopy ...................................................................................................... 5 2.3 Surface-Enhanced Raman Scattering (SERS) ............................................................... 7 2.3.1 Electromagnetic enhancement (EM) .................................................................. 8 2.3.2 Chemical enhancement (CM) ............................................................................. 9 2.4 Substrate types for SERS enhancement....................................................................... 10 2.4.1 Nanoparticles .................................................................................................... 11 2.4.2 Three-dimensional nanostructure ..................................................................... 11 2.4.3 Core-shell structure........................................................................................... 12 2.4.4 Periodic nanostructure ...................................................................................... 14 2.5 The importance of nanoscale noble metal in SERS..................................................... 15 2.6 Common SERS probes ................................................................................................ 17 2.6.1 Potential application of Crystal violet .............................................................. 17
6.2 Potential application of Rhodamine 6G............................................................ 18 V
7 Metallic Glass Nanotube Arrays (MGNT arrays)........................................................ 19 2.7.1 Unique properties of MGNT arrays.................................................................. 22 2.7.2 MGNT arrays applied in SERS application...................................................... 24
8 Metallic Nanotube Arrays (MeNTAs) ......................................................................... 26 Chapter 3 Experimental Procedure.......................................................................................... 33 3.1 Metallic Nanotube arrays (MeNTAs) fabrication of Ti64, AA and pure Au ............... 33 3.1.1 Substrate and photoresist preparations ............................................................. 35 3.1.2 Metallic thin-film deposition (laminated layers) .............................................. 36 3.1.3 Photoresist removal .......................................................................................... 37 3.2 Fabrication of MeNTAs covered in noble metal nanoparticles (AuNPs@MeNTAs) . 37 3.2.1 Substrate and photoresist preparations ............................................................. 39 3.2.2 Thin-film Metallic Glass (TFMG) deposition .................................................. 39 3.2.3 Synthesis of gold nanoparticles ........................................................................ 39 3.2.4 Photoresist removal .......................................................................................... 40 3.3 Fabrication of core-shell triangular MeNTAs.............................................................. 40 3.3.1 Substrate and photoresist preparation ............................................................... 42 3.3.2 Deposition of core-shell triangular MeNTAs ................................................... 43 3.3.3 Photoresist removal .......................................................................................... 44 3.4 Characterization of thin films ...................................................................................... 44 3.4.1 Crystallographic analysis (XRD)...................................................................... 44 3.5 Characterization of MeNTAs....................................................................................... 44 3.5.1 Composition analysis and TEM specimen preparation (FIB) .......................... 45 3.5.2 Wettability ......................................................................................................... 45 3.5.3 Elemental surface analysis (AES) .................................................................... 46 3.5.4 Microstructural analysis (TEM) ....................................................................... 46 3.6 Raman spectroscopy .................................................................................................... 46
VI

6.1 Adsorption of Crystal violet and Rhodamine 6G onto AuNPs@MeNTAs ...... 47
6.2 Adsorption of Rhodamine 6G onto triangular MeNTAs .................................. 47 Chapter 4 Results and Discussion ........................................................................................... 48 4.1 Circular MeNTAs of Ti64, AA and pure Au ................................................................ 48 4.1.1 Surface morphology (SEM).............................................................................. 48 4.1.2 Wettability (Water contact angle) ..................................................................... 49 4.1.3 Crystallographic analysis (XRD)...................................................................... 54 4.1.4 Auger analysis (Auger) ..................................................................................... 55 4.1.5 Microstructural analysis (TEM) ....................................................................... 58 4.1.6 Raman spectra for MeNTAs and films ............................................................. 67 4.2 Circular MeNTAs covered in noble metal nanoparticles (AuNPs@MeNTAs) ........... 68 4.2.1 Surface morphology (SEM) of AuNPs@MeNTAs .......................................... 68 4.2.2 Chemical composition analysis (EDS) of AuNPs@MeNTAs .......................... 71 4.2.3 Crystallographic analysis (XRD) of AuNPs@MeNTAs................................... 72 4.2.4 Raman spectra of different structure effect....................................................... 73 4.2.5 Limit of detection (LOD) of AuNPs@MeNTAs .............................................. 74 4.2.6 Reproducibility of AuNPs@MeNTAs .............................................................. 77 4.2.7 Raman mapping of AuNPs@MeNTAs ............................................................. 79 4.3 Core-shell triangular MeNTAs .................................................................................... 80 4.3.1 Surface morphology (SEM).............................................................................. 80 4.3.2 Crystallographic analysis (XRD)...................................................................... 84 4.3.3 Raman spectra of different nanotube shapes .................................................... 85 4.3.4 Raman spectra of triangular MeNTAs with different detection areas .............. 86 4.3.5 Raman spectra of triangular MeNTAs with different compositions ................. 88 4.3.6 Raman spectra of triangular MeNTAs with different outer diameters ............. 91 4.3.7 Limit of detection (LOD) of core-shell triangular MeNTAs ............................ 93
VII

3.8 Reproducibility of core-shell triangular MeNTAs............................................ 96
3.9 Raman mapping of core-shell triangular MeNTAs........................................... 97 Chapter 5 Conclusions............................................................................................................. 99 References ................................................................................................................................ 101

                                

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