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http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/54199完整後設資料紀錄
| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 林江珍 | |
| dc.contributor.author | Hsiao-Chu Lin | en |
| dc.contributor.author | 林筱筑 | zh_TW |
| dc.date.accessioned | 2021-06-16T02:44:21Z | - |
| dc.date.available | 2020-07-22 | |
| dc.date.copyright | 2015-07-22 | |
| dc.date.issued | 2015 | |
| dc.date.submitted | 2015-07-20 | |
| dc.identifier.citation | 1.7 Reference
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/54199 | - |
| dc.description.abstract | 本研究主要在於探討利用酯化反應及麥克加成反應製備新穎的起始劑，並再以溶膠–凝膠法進行共價鍵結於脫層型奈米矽片上，進一步利用原子轉移自由基聚合法將高分子接枝於奈米矽片製備新型奈米複合材料。研究分為三部分：（1）製備新型雙親性複合材料矽片－聚異丙基丙烯醯胺並探討其界面性質的變化。（2）導入奈米銀粒子於矽片－聚異丙基丙烯醯胺中，利用其溫度感應性質對於不同細菌的抗菌或偵測研究。（3）製備矽片－聚六乙基甲基丙烯酸酯並導入具螢光之化合物作為螢光偵測細菌之新型複合材料研究。以上各部分主要探討如下：
第一部分為將高分子聚異丙基丙烯醯胺接枝於奈米矽片製備新型雙親性奈米複合材料。研究中發現由於高分子與矽片有親疏水差異因而造成如同界面活性劑的界面現象，而製備不同接枝密度或改變起始劑之結構會影響分子間或分子內作用力的變化，進而改變其界面性質。當高分子接枝密度大時，因為分子間團聚力較大導致臨界微胞濃度上升。而改變起始劑接枝構型由一個變為兩個接枝點時，也會造成高分子間團聚力提高而使臨界微胞濃度上升。此研究利用表面張力、粒徑測量觀察其差異，同時藉由分子模擬亦可證明其結果。 第二部分是將還原奈米銀粒子於矽片－聚異丙基丙烯醯胺中。由結果顯示銀粒子大小具均一性約8奈米且穩定貼附於矽片表面，此結果可經由TEM觀察。銀粒子/矽片－聚異丙基丙烯醯胺中仍保有最低臨界溶解溫度32－33 oC，可由UV-vis及DSC觀察。利用此複合材料的溫感特性，可以用來辨識格蘭氏陽性菌及陰性菌的不同。在高於最低臨界溶解溫度的37 oC時，複合材料較為疏水所以容易與表面疏水的格蘭氏陰性菌親和，反之，當溫度為28 oC時複合材料轉為親水性而與表面親水的格蘭性楊氏菌親和。此結果在抗菌及表面增強拉曼光譜可以驗證。此新型複合材料可作為偵測不同細菌之研究。 第三部分是延續第一部分之合成方法製備矽片－聚六乙基甲基丙烯酸酯。利用縮合反應將具有螢光之化合物鍵結於高分子鏈段製備出新型具有螢光性質的奈米複合材料。利用矽片表面的離子與細菌間的物理捕捉效應，進而可以利用螢光的強弱變化偵測細菌含量。由SEM可以觀察矽片貼附於細菌表面。利用離子交換法改質矽片所製備之螢光矽片則因為離子交換之螢光化合物無法穩定接於矽片上，而無法有效利用於細菌的偵測。由螢光光譜可以觀察兩者螢光強弱變化的差異。此新型螢光複合材料可應用於偵測細菌。 | zh_TW |
| dc.description.abstract | Nanoscale silicate platelets (NSP) were derived from the exfoliation of naturally occurring sodium montmorillonite clay. The silicate platelets were modified with two different polymers via a novel initiator covalently bonded to the edge of NSP by a sol–gel reaction and atom transfer radical polymerization (ATRP) to afford the new class of nanohybrids. In this study, we grafted poly(N-isopropylacrylamide) (PNiPAAm) onto the edge of NSP through the covalent bonding with single- or double-headed linkers to prepare the NSP-PNiPAAm nanohybrids. By tailoring the architecture of the linker and controlling the number of grafted linkers, we were able to prepare NSP-PNiPAAm of varios grafting densities. The inherent ionic character of NSP and the organic moieties of isopropyl amide in PNiPAAm impart surfactant-like properties to the nanohybrids. Surface tension and particle size measurements were used to determine the critical micelle concentration (CMC) of the nanohybrids. The CMC can be tailored by adjusting the densities and architectures of the linkers. The NSP-PNiPAAm nanohybrids from single-headed linkers are loosely packed and can easily expand in water to faciliate inter-hybrid interactions to render a low CMC. In contrast, the nanohybrids from double-headed linkers enhance intra-hybrid interactions, thus exhibiting a higher CMC. The simulation results were found to be in a good agreement with the experimental observations.
We further introduced silver nanoparticles (AgNPs) onto NSP-PNiPAAm. The generated AgNPs had an average diameter of 8 nm with a narrow size distribution. The AgNP/NSP-PNiPAAm exhibited the property of lowest critical solution temperature (LCST) at 32 oC, which was similar to the LCST of the NSP-PNiPAAm precursor. This is a clear indication of AgNPs attachment on the NSP surface rather than with PNiPAAm organic chains. The strong embedment between AgNPs and NSP was evidenced by transmission electron microscopic (TEM) and LCST thermal cycles between 28-37 oC monitored by ultraviolet-visible spectrophotometry (UV-vis). At 37 oC, the nanohybrids and E. coli give stronger SERS intensities and hydrophobic interaction than the hydrophilic B. subtilis counterparts. In contrast at 28 oC, the nanohybrids interact with hydrophilic B. subtilis, thus giving a relatively strong SERS intensities. Similar results were also observed in their antibacterial ability. It could be thus anticipated that the new AgNP/NSP-PNiPAAm hybrids have good potentials to serve as biosensors and antibacterial materials. We have also synthesized new fluorescent nanohybrids via tethering poly(hydroxyethyl methacrylate) pendants (HEMA) onto NSP through a sol-gel and living polymerization and by a further modification of the pendants with a nathphalimide-type fluorescence compound. The fluorescent NSP-PHEMA-HA was characterized for their photoluminescence (PL) and bacterial trapping properties from NSP’s affinity toward the surface of bacteria. In addition, the investigation of PL emission revealed that the fluorescent NSP hybrids could be applicable in bacteria detection. The fluorescent NSP hybrids are proposed for the biosensor applications for the combined features of photoluminescence and physical trapping for bacteria. | en |
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| dc.description.tableofcontents | Index
摘要 I Abstract III List of Figures X List of Tables XIV List of Schemes XV Chapter 1 Introduction 1 1.1 Introduction of nanomaterials 1 1.2 Fundamental structure of layeren clays 3 1.3 Organic modification of clay by intercalation and exfoliation 5 1.3.1 Ionic exchange method 5 1.3.2 Modification by covalent bonding 7 1.4 Fundamental properties of Nanoscale silicate platelet (NSP) 9 1.5 Atom Transfer Radical Polymerization (ATRP) 12 1.6 Clay/polymer nanocomposite 14 1.7 Reference 16 Chapter 2 Effect of grafting architecture on the surface-like behavior of clay-poly(NiPAAm) nanohybrids 24 2.1 Introduction 25 2.2 Experimental section 30 2.2.1 Materials 30 2.2.2 Synthesis of the mono-bromr-triethoxysilane (MBTES) and bis-bromo-triethoxysilane (BBTES) linkers with bromide and triethoxysilane functionalities 30 2.2.3 Preparation of different NSP-linker as initiator 32 2.2.4 Atom transfer radical polymerization grafting of PNiPAAm 33 2.2.5 Characterization and analytical instruments 34 2.3 Simulation model and method 36 2.4 Results and discussion 38 2.4.1 Synthesis of the mono-bromr-triethoxysilane (MBTES) and bis-bromo-triethoxysilane (BBTES) linkers with bromide and triethoxysilane functionalities 38 2.4.2 Tethering the different initiator to NSP 39 2.4.3 PNiPAAm grafting via ATRP 42 2.4.4 Comparison of CMC between pure PNiPAAm and NSP-PNiPAAm hybrids 43 2.4.5 Effect of grafting architecture on the CMCs of NSP-PNiPAAm hybrids 45 2.4.6 CMC from particle size measurement of NSP-PNiPAAm hybrids 47 2.4.7 Comparison between simulation and experimental results 49 2.5 Conclusion 51 2.6 Reference 53 Chapter 3 Synthesizing Tri-Component Nanohybrids of Silver Nanoparticle, Silicate Nanoplatelet and Thermo-Responsive PNiPAAm for the Antimicrobial Applications 57 3.1 Introduction 58 3.2 Experimental section 60 3.2.1 Materials 60 3.2.2 Synthesis of dual-linker with bromide and triethoxysilane functionality 60 3.2.3 General procedure for the preparation of NSP-linker as an initiator 61 3.2.4 Atom transfer redical polymerization grafting of PNiPAAm to NSP 61 3.2.5 General procedure for the preparation of AgNP/NSP-PNiPAAm dispersion 62 3.2.6 Preparation of bacterial cultures 63 3.2.7 Bacteria growth and inhibition assay 63 3.2.8 SERS detection 63 3.2.9 Characterization 64 3.3 Results and discussion 65 3.3.1 Synthesis of AgNP/NSP-PNiPAAm nanohybrids 65 3.3.2 Analysis of AgNP/NSP-PNiPAAm nanohybrids 67 3.3.3 Interaction between AgNPs and the surface of NSP-physical blending 71 3.3.4 The influence of the thermo-responsiveness of NSP-PNiPAAm hybrid on AgNPs 74 3.3.5 Selective antibacterial activity by thermo-responsive effect of AgNP/NSP-PNiPAAm nanohybrids 75 3.3.6 Selective SERS detecting capability by thermo-responsive effect of agNP/NSP-PNiPAAm nanohybrids 78 3.4 Conclusion 80 3.5 Reference 81 Chapter 4 Interaction of Novel Fluorescent Nanoscale Ionic Silicate Platelets with Biomaterials for Biosensors 84 4.1 Introduction 85 4.2 Experimental section 88 4.2.1 Materials 88 4.2.2 Synthesis of dual-linker wirh bromide and triethoxysilane functionality 89 4.2.3 Preparation of NSP-linker as an initiator 89 4.2.4 Atom transfer radical polymerization grafting of PHEMA to NSP 90 4.2.5 Preparation of fluorescent NSP-PHEMA-HA 90 4.2.6 Ionic exchange of Na+-NSP by 1-aminopyrene-salts 92 4.2.7 Prepartion of bacterial cultures 92 4.2.8 SEM observation experiments of NSP-PHEMA-HA with bacterial 92 4.2.9 Characterization 93 4.3 Results and discussion 94 4.3.1 Synthesis and characterization of NSP-PHEMA-HA 94 4.3.2 Synthesis and characterization of NSP-Pyrene 97 4.3.3 Interaction between NSP hybrids and bacteria 99 4.3.4 Zeta potential of NSP and NSP-Pyrene 101 4.3.5 Physical Trapping and detection of NSP-PHEMA-HA 102 4.4 Conclusion 106 4.4 Reference 107 Chapter 5 Summary 113 Appendix 114 List of Figures Figure 1.1. Morphology of nanomaterials (A) spherical (silver nanoparticles); (B) rod/fiber-like (carbon nanotubes); (C) layer/lamellar (nature clays). 1 Figure 1.2. Structure of sodium montmorillonite 4 Figure 1.3. Representation of Na+-MMT intercalateion by hydrophilic and hydrophobic poly(oxyalkylene)-diamine salts with the same molecular weight. 6 Figure 1.4. The condensation of tetraethoxysilane (TEOS) in sol-gel processs 8 Figure 1.5. (a) Synthesis of AMO polyamines from hydrophobic and hydrophilic POA-diamine, p-cresol, and formaldehyde. (b) Conceptual representations of an intercalated silicate stack and exfoliated platelets in association with the polyamines at different amine/H+ ratios 9 Figure 1.6. Synthesis process of NSP 10 Figure 1.7. (a) Preparation of NSP material by the exfoliation of layered Na+-MMT in water and its physical properties. (b) TEM and (c and d) AFM micrographs of exfoliated silicate platelets suspended in water (0.1 wt%). 11 Figure 1.8. General ATRP Reaction (A) Initiation. (B) Equilibrium with dormant species. (C) Propagation 12 Figure 1.9. Methods of incorporating functionality into polymers using ATRP 13 Figure 1.10. (a) Schematic representation of the organic/inorganic network in the NC gel, which consists of uniformly dispersed (exfoliated) inorganic clay sheets and two primary types of flexible polymer chains, χ and g, grafted to two neighboring clay sheets and one clay sheet, respectively. (b) All NC gels exhibit extraordinary mechanical toughness. 15 Figure 1.11. (a) Schematic representation of the internal architecture of the PVA/MMT nanocomposite (picture shows 8 bilayers). (b) Close-up of the cross section showing the separation of layers. (c) Free-standing, 300-bilayer PVA/MMT composite film showing high flexibility and transparency. The lower image was taken at an angle to show diffraction colors. 15 Figure 2.1. FTIR spectra of HEA, bromo-terminated acrylate, and mono-bromo-triethoxysilane..... 39 Figure 2.2. FTIR spectra of NSP-BBTES and NSP-PNiPAAm. 41 Figure 2.3. Surface tension of PNiPAAm and NSP-PNiPAAms at different concentrations..…………….. 44 Figure 2.4. Conceptual diagrams of NSP-PNiPAAms in water 46 Figure 2.5. Surface tension of NSP-PNiPAAm-H1 versus time 47 Figure 2.6. Simulation results of the CMCs for (a) hybrids with different grafting density and (b) hybrids using different types of linkers. 50 Figure 3.1. (a) Monitoring the formation dynamics of AgNPs from the reduction of Ag+ ions to Ag0 at the presence of NSP-PNiPAAm hybrid (WA/N-P = 7/93) by using UV spectrophotometry. (b) UV-Vis spectra of AgNP/NSP-PNiPAAm nanohybrids at different WA/N-P.t.... 68 Figure 3.2. TEM images of (a) AgNP/ PNiPAAm (WA/P = 7/93), (b) AgNP/ NSP (WA/N = 7/93), (c), (d), (e), and (f) AgNP/ NSP-PNiPAAm (WA/N-P = 3/97, 5/95, 7/93, and 10/90, respectively), and (g) cross-section of AgNP/ NSP-PNiPAAm (WA/N-P = 7/93). 70 Figure 3.3. UV spectra of AgNP/NSP-PNiPAAm nanohybrids and physical blend of AgNP/NSP/PNiPAAm at 28 and 37 oC. 72 Figure 3.4. (a) LCST of AgNP/NSP-PNiPAAm, NSP-PNiPAAm and NSP. (b) DSC analysis of AgNP/NSP-PNiPAAm and NSP-PNiPAAm..…………….. 73 Figure 3.5. UV-vis spectra of reversible absorption of AgNPs on AgNP.NSP-PNiPAAm for several heating-cooling cycles 75 Figure 3.6. Comparison on the antibacterial ability between AgNP/NSP-PNiPAAm (WA/N-P = 7/93) and AgNP/ NSP against (a) E. Coli and (b) B. subtilis at 28 and 37 oC. 77 Figure 3.7. SERS intensity of AgNP/NSP-PNiPAAm nanohybrids against E. coli (hydrophobic bacteria) at (a) 28 and (b) 37 oC, and AgNP/NSP-PNiPAAm nanohybrids against B. subtilis (hydrophilic bacteria) at (c) 28 and (d) 37 oC 79 Figure 4.1. FTIR spectra of NSP-PHEMA-HA and NSP-Pyrene..... 95 Figure 4.2. (a) UV–vis spectra and photoluminescent spectra in different excited wavelength of NSP-PHEMA-HA. (b) The photoluminescent spectra of NSP-PHEMA-HA in different concentration. The inserted part were the photos of compounds under the UV light.. 96 Figure 4.3. (a) UV–vis spectra and photoluminescent spectra in different excited wavelength of NSP-pyrene. (b) The photoluminescent spectra of NSP-pyrene in different concentration. The inserted part were the photos of compounds under the UV light. 98 Figure 4.4. Photoluminescent spectra of NSP-PHEMA-HA and NSP-pyrene with different bacteria respectively. In which, a is NSP-PHEMA-HA (50 ppm) only, b is with 107 CFU/mL E. coli or S. aureus, c is with 106 CFU/mL , d is with 105 CFU/mL and e is 107 CFU/mL E. coli or S. aureus only..…………….. 100 Figure 4.5. Zata potential of NSP and NSP-pyrene in different pH. 102 Figure 4.6. SEM micrographs of original (a) E. coli and (b) S. aureus and after treatment with NSP-PHEMA-HA (0.005 wt %) over a 1 h ((c) for E coli and (d) for S. aureus). 104 List of Tables Table 2.1. Characterization of the NSP-linkers 42 Table 2.2. Particle size of NSP-PNiPAAM hybrids at different concentrations 48 List of Schemes Scheme 2.1. Synthesis of the linker by esterification and Michael addition 31 Scheme 2.2. (a) Linkers tethering onto NSP edges by sol-gel reaction; (b) Conceptual diagram of NSP- PNiPAAm formation by the ATRP “grafting from” method and morphological transformation at LCST. 34 Scheme 3.1. Conceptual diagrams of NSP-PNiPAAm by ATRP and in-situ reduction of Ag+ to AgNPs to afford the thermoresponsive AgNP/NSP-PNiPAAm. 66 Scheme 3.2. Conceptual diagrams of AgNP/NSP-PNiPAAm interaction with different bacteria at 28 and 37 oC.. 79 Scheme 4.1. Conceptual diagram of preparation of NSP-PHEMA-HA by sol-gel and ATRP 91 Scheme 4.2. Conceptual diagram of preparation of NSP-Pyrene by ionic exchanging 97 Scheme 4.3. Conceptual diagram of the mechanism of NSP-PHEMA-HA and NSP-pyrene reacted with bacteria at the detected environment in pH= 7. 105 | |
| dc.language.iso | en | |
| dc.title | 原子轉移自由基聚合應用於奈米矽片接枝高分子及其介面、螢光感測、抗菌性質之探討 | zh_TW |
| dc.title | Studies on Polymers Grafting from Exfoliated Silicate Nanoplatelets via Atom Transfer Radical Polymerization and Applications of Surface Properties, Fluorescent Sensors and Antibacterial Abilities | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 103-2 | |
| dc.description.degree | 博士 | |
| dc.contributor.oralexamcommittee | 謝國煌,諶玉真,何永盛,戴憲弘,鄭如忠 | |
| dc.subject.keyword | 原子轉移自由基聚合,奈米矽片,聚異丙基丙烯醯胺,臨界微胞濃度,奈米銀粒子,最低臨界溶解溫度,聚六乙基甲基丙烯酸酯,物理捕捉效應,螢光偵測, | zh_TW |
| dc.subject.keyword | atom transfer radical polymerization,nano silicate platelets,poly(N-isopropylacrylamide),critical micelle concentrations,silver nanoparticles,lowest critical solution temperature,poly(hydroxyethyl methacrylate),physical trapping,fluorescent sensors, | en |
| dc.relation.page | 116 | |
| dc.rights.note | 有償授權 | |
| dc.date.accepted | 2015-07-20 | |
| dc.contributor.author-college | 工學院 | zh_TW |
| dc.contributor.author-dept | 高分子科學與工程學研究所 | zh_TW |
| 顯示於系所單位： | 高分子科學與工程學研究所 | |
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