貴金屬奈米粒子/二維奈米片混成材料之製備及其表面增強拉曼光譜之應用

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研究生：	李彥蓁 Yen-Chen Lee
論文名稱：	貴金屬奈米粒子/二維奈米片混成材料之製備及其表面增強拉曼光譜之應用 Fabrication of Precious Metal Nanoparticles and Two-dimensional Nanoplatelets Hybrids for Surface-Enhanced Raman Spectroscopy Applications
指導教授：	邱智瑋 Chih-Wei Chiu
口試委員:	邱顯堂游進陽鄭智嘉鄭如忠蔡燕鈴劉定宇
學位類別：	博士 Doctor
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：	2020
畢業學年度：	108
語文別：	英文
論文頁數：	173
中文關鍵詞：	奈米金粒子、表面增強拉曼散射、黏土、靜電紡絲、石墨烯、腺嘌呤
外文關鍵詞：	AuNPs, SERS, Clay, Graphene, Electrospinning, Adenine
相關次數：	點閱：364 下載：0
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表面增強拉曼散射(Surface Enhanced Raman Scattering，縮寫為SERS)可以廣泛應用於生物、醫藥、電化學、食品科學、環境工程等領域，並可偵測各種的有機生物分子。其原理是利用粗糙的貴金屬表面，例如奈米金或銀粒子，可以將拉曼散射訊號放大一百萬倍，有這高靈敏度、無單一性及快速的好處，加上近十年奈米技術的進步，使得其發展迅速。然而，一般市面上所製備的底板大多面積小、成本高及製成不易，為了解決這些問題，本研究中使用簡單的化學還原法複合二維材料產生三維熱點，作為大面積高靈敏度的表面增強拉曼散射底版。
第一部分利用無機的奈米矽片(黏土)良好的陽離子交換的能力，可以用以穩定奈米金粒子，使用穿透式電子顯微鏡（Transmission Electron Microscopy，TEM）成功證實了使用不同尺寸的黏土(laponite、Na + -MMT、雲母)來穩定奈米金粒子落在25 - 30nm並且有形狀的相似性。另一方面，黏土也具有高吸水性，可以用以捕捉待測分子，我們使用此底板做拉曼散射的快篩，用來檢測常見的染料直接藍200 (Direct Blue 200)、DNA的腺嘌呤 (Adenine)及農藥的百草枯 (Paraquat)，都可達到三維的熱點效應，其極限濃度達10-8M以上，大約為0.01ppm以下，增強因子 (Enhancement Factor, EF)為7 × 105。
第二部分設計柔性便於攜帶的拉曼散射基材，以生物可降解的聚乙烯醇(Polyvinyl alcohol, PVA)作為靜電紡絲的支架，使用同軸靜電紡絲技術，將奈米金粒子均勻的分佈在奈米纖維表面上，製備殼/核奈米金粒子@人造黏土/聚乙烯醇奈米纖維膜。其纖維膜因纖維隨機沉積而具有三維的纖維結構。比較與傳統的靜電紡絲技術，所需的金含量濃度低，且可以接觸到待測物，進而展現出較高的拉曼散射訊號達到10-7M，同時因減少奈米金粒子對纖維結構的破壞，其極限抗拉強度提升1.5倍。拉曼檢測中，其在直接藍200展現出10-8M的極限濃度及增強因子2.5× 105，對百草枯和腺嘌呤的極限檢測濃度都有10-7M的極限濃度，展現出良好的再現性。
第三部分，思考是否可以在二維材料本身就用可以用以增強拉曼散射訊號，故選用了石墨烯材料。其分散劑的設計是以親水/疏水性三團聯共聚物和氧化石墨烯（Graphene Oxide，GO）所組成的有機/無機奈米混成分散劑來穩定奈米銀粒子(AuNPs)。透射電子顯微鏡測量證實了所得的AgNPs具有〜15nm的窄尺寸分佈。這些AgNPs吸附在氧化石墨烯的兩側上，形成AgNPs /共聚物/ GO的複合材料。氧化石墨烯提供1-5 nm的厚度，使得奈米銀粒子間有一定的距離，形成三維熱點。用於表面增強拉曼散射，對腺嘌呤的增強因子為1.2×105。
第四部份，因奈米銀粒子活性高且易氧化，使應用受限，故使用奈米金粒子為材料，以奈米金粒子/共聚物/石墨烯複合材料底板做為表面增強拉曼材料。經由穿透式電子顯微鏡觀察可以知道奈米金粒子粒徑介於25 nm至35 nm的窄粒徑範圍。進一步將AuNPs/GO分散液利用溶液滴塗法沉積在鋁基板上，因二維的氧化石墨烯具有自組裝特性，使得奈米金粒子/氧化石墨烯混合物形成規則的層狀排列，成為大面積拉曼基板，並以300℃退火2小時移除分散劑後，通過掃描式電子顯微鏡（Scanning Electron Microscopy，SEM）測量證實，因二維GO奈米片的穩定控制金奈米顆粒尺寸僅成長至40 nm左右。且因氧化石墨烯的厚度約為1~5 nm間，使得AuNPs的顆粒間距小而產生良好的三維（3D）熱點效應。最後對具有高螢光性質的常見染料羅丹明6G（Rhodamine 6G，R6G）進行表面增強拉曼散射的檢測，其增強因子（Enhancement Factor，EF）呈現極佳的靈敏度，約為2.7 × 107。因此，奈米金/氧化石墨烯奈米片作為SERS基底，且其為可撓且大面積的基板材料，在環境檢測應用中具有很大的潛力。

Surface Enhanced Raman Scattering (SERS) can be widely used in biology, medicine, electrochemistry, food science, environmental engineering and other fields. It can detect a variety of organic biological molecules. The principle of SERS is to use a rough precious metal surface, such as gold or silver nanoparticles, to amplify the Raman scattering signal more than million times. SERS is good at its’ high sensitivity and wide application. With the progress of nanotechnology, SERS develop rapidly. However, the substrate in market are almost small in area with high cost and difficult on manufacture. In order to solve these problems, a simple chemical reduction method was used in this study to generate three-dimensional hotspots by compositing two-dimensional materials as a large-area high-sensitivity Surface enhancement Raman Scattering substrate.
In the first part, use the cation exchange capacity from clay to stable the gold nanoparticle (AuNPs). The use of various dimensions of clay to stabilize the AuNPs, such as laponite, Na+-MMT, mica, that forming the narrow particle diameter range between 25–30 nm was successfully confirmed by transmission electron microscopy (TEM) measurement. In addition, the SERS substrate could be applied to biological, environmental, and food safety that measured by small molecules included adenine of DNA, direct blue of dye, paraquat of pesticide and the sensitivity was improved with an enhancement factor (EF) of 9.3 × 105 and limit of detection (LOD) of 10-9 M.
In the second part, make the bendable and environmentally friendly substrates prepared by coaxial electrospinning technique composed of core/shell gold nanoparticles(AuNPs) with clay nanoplateles synthesized by sodium citrate reducing and poly(vinyl alcohol) nanosphere hybrids as core fluid. The core/shell hybrid nanofiber membrane has the three-dimensional (3D) networked formation which has homogeneous AuNPs distribution insides layer-by-layer deposited randomly. Transmission electron microscopy (TEM) observation showed the core/shell structure and the AuNPs embedded into the surface of nanofiber and oriented along their axes while getting the better mechanical properties which confirmed by tensile test. Compare with traditional electrospinning, the core-shell membranes can easier contact with molecular and enhance the Raman intensity. Detecting dye (Direct Blue 200) and herbicide (paraquat) showed good enhancement factor (EF) more than 10-5 and LOD is 10-8 M and 10-7M respectively. In additional, the high EF and LOD more than 10-7M found in detecting DNA (adenine molecule), the basic component of life, and the high relative standard deviations (RSD) of different contents adenine was about 92.3% which can confirm the possibility in bio-tech.
In the third part, select the two-dimensional materials such as graphene oxide (GO) to improve the Raman signal. Silver nanoparticles (AgNPs) are well dispersed in an organic/inorganic nanohybrid surfactant consisting of an amphiphilic triblock copolymer and graphene oxide (GO) as Raman substrate. AgNPs had a narrow size distribution of ∼15 nm confirmed by TEM measurements. These AgNPs were adsorbed on both sides of the GO nanosheets, forming controllable nanodispersions of the AgNPs/copolymer/GO hybrid. A facile method for fabricating the desired nanohybrid SERS films was therefore developed by immobilizing spherical AgNPs with a narrow size distribution on both sides of the 3−5 nm-thick GO nanosheets, which afforded 1−5 nm interparticle distances between the AgNPs. Furthermore, the hybrid substrate films formed three-dimensional (3D) hot-junctions and exhibited an SERS enhancement factor (EF) of 1.2 × 105 toward adenine molecules from DNA, which served as a model biomolecular target.
In the fourth part, because of the oxidation reaction from AgNPs, use the AuNPs as materials. The narrow particle diameter range between 25nm to 35nm was confirmed by transmission electron microscopy (TEM) measurements. After the annealing at 300 ℃ for 2hrs to remove the dispersant, the gold nanoparticles grew up to around 40nm confirmed by scanning electron microscopy (SEM) measurements. These AuNPs were adsorbed on both sides of the GO nanosheets to produce the three-dimensional (3D) hot-junctions which afforded 1-5nm interparticle distances between the AuNPs by the thickness from graphene oxide. On the other side of the great self-assembling property of the graphene oxide that the AuNPs/GO hybrid become regular layered arrangement to be large area Raman substrate and exhibited an SERS enhancement factor (EF) of 2.7 × 107 toward adenine molecules from DNA, which served as a model biomolecular target. Therefore, the AuNPs/GO nanosheets as SERS substrates have great potential in biosensor technology applications because they are flexible, free-standing, highly stable and large-scale.

Chinese Abstract    I
Abstract    III
Acknowledgement    VI
Contents    VII
Figure    X
Tables    XV
Chapter 1    Introduction    1
1    Prolegomena    1
2    Purpose    2
Chapter 2    Review    3
1    Raman Scattering    3
1.1    History and Basic Principles    3
1.2    Surface Enhance Raman Scattering    3
1.3    Application    7
2    Nanotechnology    7
2.1    Dispersion of nanomaterials    9
2.2    Nano-metal    10
2.3    Clay    13
2.4    Graphene    16
3    Electrospinning    22
3.1    Electrospinning Device    23
3.2    Processing Parameters of Electrospinning    24
3.3    Electrospinning technology use as SERS substrate    26
4    Reference    28
Chapter 3    Experiment Section    35
1    Flow chart    35
2    Materials    37
3    Instruments    40
Chapter 4    Immobilization and 3D Hot-Junction Formation of Gold Nanoparticles on Two-Dimensional Silicate Nanoplatelets as Substrates for High-Efficiency Surface-Enhanced Raman Scattering Detection    42
1    Abstract    42
2    Introduction    42
3    Experiment section    44
3.1    Preparation of AuNPs /clay Nanocomposites Hybrid Suspensions    44
3.2    Preparation of the SERS Samples    45
4    Results and discussion    46
4.1    Dispersion Mechanism for the Gold Nanoparticles/Clay Nanoplatelet    46
4.2    Comparison of the Stabilization of AuNPs in Different Weight Ratio of Clay as Inorganic Stabilizer Agent    50
4.3    The Raman Shift of SERS Samples in AuNPs/Clay Hybrids    58
5    Summary    64
6    References    65
Chapter 5    Spherical Nanohybrids of Core-Shell Gold Nanoparticles-Silican Nanoplatelets@Poly(Vinyl Alcohol) by coaxial electrospinning technique as High-Efficiency SERS Substrates    70
1    Abstract    70
2    Introduction    70
3    Experiment section    73
3.1    Preparation of AuNPs /clay Nanocomposites hybrid suspensions    73
3.2    Fabrication of the AuNPs/Laponite@PVA Composite Nanofiber membrance by Co-Electrospinning Technique    73
4    Results and discussion    74
4.1    Fabrication and dispersion for the Gold Nanoparticles/Clay Nanoplatelet    74
4.2    Fabrication and Characterization of Core-Shell Structured Nanofibers with AuNPs Loaded Shell    77
4.3    Application of Gold Nanoparticles/Silicate@Poly(Vinyl Alcohol) membranes as SERS Substrates    85
5    Summary    92
6    References    93
Chapter 6    Controllable 3D Hot-Junctions of Silver Nanoparticles Stabilized by Amphiphilic Tri-block Copolymer/Graphene Oxide Hybrid Surfactants for Use as Surface-Enhanced Raman Scattering Substrates    97
1    Abstract    97
2    Introduction    98
3    Experiment section    100
3.1    Synthesis and characterization of triblock copolymer as a dispersant tri-Block Copolymer as a Dispersant    100
3.2    Preparation of immobilized AgNPs on copolymer/GO nanohybrid surfactants    100
3.3    Preparation of the SERS Samples    101
4    Results and Discussion    102
4.1    Dispersion Mechanism for the AgNPs/Copolymer/GO Nanohybrids.    102
4.2    Comparison of the Stabilization of AgNPs by Organic Copolymer Dispersants and Organic/Inorganic Copolymer/GO Hybrid Dispersants    104
4.3    3D Hot-Junctions in AgNPs/Copolymer/GO Hybrids    110
5    Summary    116
6    References    117
Chapter 7    Fabrication and Layer-by-Layer Self-Assembling of Gold Nanoparticles Stabilized by Organic/Inorganic Hybrid Dispersants for Large Area and Highly Sensitive SERS Detection    124
1    Abstract    124
2    Introduction    124
3    Experiment Section    127
3.1    Preparation of Immobilized AuNPs on Copolymer/Graphene oxide Composite Hybrids    127
3.2    Preparation of Large Area SERS Substrate    127
4    Results and Discussion    128
4.1    Dispersion Mechanism for the AgNPs/Copolymer/GO Nanohybrids.    128
4.2    Fabrication and Dispersion for the Gold Nanoparticles and Copolymer    131
4.3    Fabrication of the Gold anoparticles/Copolymer/Graphene oxide    133
4.4    The Raman Substrate with Large Area    141
5    Summary    145
6    Reference    146
Chapter 8    Conclusion    151
Appendix    153
1    Publication List    153
2    Award Record    155
                                

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