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http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/22197完整後設資料紀錄
| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 林唯芳(Wei-Fang Su) | |
| dc.contributor.author | Chien-Chih Lin | en |
| dc.contributor.author | 林建志 | zh_TW |
| dc.date.accessioned | 2021-06-08T04:13:40Z | - |
| dc.date.copyright | 2010-08-16 | |
| dc.date.issued | 2010 | |
| dc.date.submitted | 2010-08-15 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/22197 | - |
| dc.description.abstract | 本論文致力於高分子-二氧化矽奈米粒子製作奈米複材、物性與化性的研究，包含三個部份。第一部份為奈米相轉移的量測，第二部份為奈米粒子大小及高分子化學種類對奈米複材物性的影響，第三部份研發新穎的具超疏水及低水氣穿透性之奈米複材。我們發現當奈米複合材料中的奈米粒子濃度達到透路限度(percolation threshold)時，我們無法以傳統宏觀的熱示差掃瞄卡量計(DSC)或是熱機械分析儀(TMA)量測到複合材料的玻璃轉移溫度。因此，我們建立一種新的奈米複合材料的量測方法 – 藉由臨場可變溫式原子力顯微鏡儀器(in situ thermal AFM)來即時觀察奈米複合材料的高分子鏈段因受熱而產生的奈米相轉移(nanophase transition)現象，進而找出奈米複合材料的表面玻璃轉移溫度(Tg, surface)。而當奈米複合材料中的二氧化矽奈米粒子含量達到透路限度(percolation threshold)時，不論是改變有機成份的化學結構，抑或是改變無機成份的奈米粒子顆粒大小時，最終複合材料整體的熱性質及機械性質均會有明顯非線性的變化量產生。最後，我們合成出氟化醯酯壓克力作為有機成份的主體，添加二氧化矽奈米粒子來補強高分子材料的耐熱及機械性質，開發出無溶劑紫外光固化的有機無機混成材料，控制其奈米區域的大小可以得到超疏水的性質，氟化醯酯的組成使材料具有極佳的透光性及極低的透水性，可以應用在光波導元件、發光二極體、太陽能電池元件封裝及牙科填補材料等多方面的用途上。 | zh_TW |
| dc.description.abstract | This thesis is devoted to polymer-silica nanocomposites to study its physical and chemical properties. It contains three parts, the first part is to monitor the nanophase transition of the nanocomposites, the second part is to discuss effects of nanoparticle sizes and type of polymer chemical structures on the properties of nanocomposites, and the final part is to develop an innovative nanocomposite which has superhydrophobic and low moisture permeation properties. We have found that when the concentration of nanoparticles reaches its percolation threshold, the glass transition temperature of nanocomposite which can not be measured by to conventional macroscale thermal analytic instruments such as DSC and TMA. Therefore, we have established a methodology basis on in-situ thermal atomic force microscope to monitor the nanophase transition of the nanocomposite upon heating. When the concentration of nanoparticles reaches its percolation threshold, a dramatic increasing in thermal and mechanical properties that is universal regardless the chemical structure of polymers and the particles of the nanoparticles in the nanocomposite. Finally, we synthesize a fluoroimide acrylate as an organic component of nanocomposite, then add silica nanoparticles to reinforce the thermal stability and mechanical properties of polymer to develope a solventless photocurable nanocomposite resin system. To control the size of nanodomain can make materials have the superhydrophobic, and fluoroimide acrlate make materials have very low water vapor permeation. It has potential application in optical waveguides, light emitting diodes, device encapsulation, dental restorative materials and so on. | en |
| dc.description.provenance | Made available in DSpace on 2021-06-08T04:13:40Z (GMT). No. of bitstreams: 1 ntu-99-D92549001-1.pdf: 4673702 bytes, checksum: 30ef2f4a53239ca1e5d101ceeb4691ec (MD5) Previous issue date: 2010 | en |
| dc.description.tableofcontents | 目錄
摘要 I Abstract II 目錄 III 圖目錄 VI 第一章 緒論 1 第二章 文獻回顧 5 第三章 量測方法的建立 – In situ probe nanophase transition in nanocomposite using thermal AFM 11 3.1 前言 11 3.2 透路限度效應(Percolation threshold effect) 13 3.3 實驗 21 3.3.1 化學藥品 21 3.3.1.1 單體 21 3.3.1.2 市售二氧化矽膠體溶液 22 3.3.1.3 光起始劑 22 3.3.2 製備透過3-(三甲氧基矽基)丙基甲基丙烯酸酯(MPS)表面改質的膠體二氧化矽 23 3.3.3 改質MA-ST-M 二氧化矽溶液 23 3.3.4 製備奈米複合材料前趨物溶液 23 3.3.5 製備奈米複合材料樣品 24 3.3.6 性質分析 24 3.3.6.1 奈米硬度(Nano-indentation) 24 3.3.6.2 熱重量分析(TGA) 25 3.3.6.3 熱機械分析(TMA) 25 3.3.6.4 稜鏡偶合儀(Prism Coupler) 25 3.3.6.5 臨場可變溫式原子力顯微鏡(in situ thermal AFM) 26 3.3.6.6 處影像處理3D AFM影像轉換成黑白影像 26 3.3.6.7 由可變溫式原子力顯微鏡圖形決定複合材料的玻璃轉移溫度 27 3.4 結果與討論 27 3.5 結論 36 第四章 二氧化矽含量與粒徑大小對奈米複材物性的非線性相關性 37 4.1 前言 37 4.2 實驗 39 4.2.1 化學藥品 39 4.2.1.1 市售二氧化矽膠體溶液 39 4.2.1.2 二氧化矽前趨物 40 4.2.1.3 單體 40 4.2.1.4 聚合物 41 4.2.1.5 偶合劑 41 4.2.1.6 光起始劑 42 4.2.2 製備透過3-(三甲氧基矽基)丙基甲基丙烯酸酯(3-(trimethoxysilyl)propyl methacrylate, MPS)表面改質的膠體二氧化矽 42 4.2.2.1 改質MA-ST-M 二氧化矽溶液 42 4.2.3 製備透過三甲基乙氧基矽(Trimethyl ethoxysilane, TMES)表面改質的膠體二氧化矽 43 4.2.3.1 改質粒徑大小不同的二氧化矽溶液 43 4.2.4 合成單一粒徑二氧化矽粒子 43 4.2.5 製備奈米複合材料前趨物溶液 44 4.2.6 製備奈米複合材料樣品 47 4.2.7 性質分析 48 4.2.7.1 傅氏轉換紅外線光譜(FT-IR) 48 4.2.7.2 奈米硬度(Nano-indentation) 49 4.2.7.3 場發射電子掃瞄顯微鏡(FE-SEM) 52 4.3 結果與討論 52 4.4 結論 69 第五章 具有高疏水性及低透濕性poly(fluoroimide acrylate)/SiO2奈米複材之無溶劑型光聚合樹脂 70 5.1 前言 70 5.2 實驗 71 5.2.1 化學藥品 71 5.2.1.1 溶劑 71 5.2.1.2 單體 71 5.2.1.3 市售二氧化矽膠體溶液 74 5.2.1.4 催化劑 74 5.2.1.5 光起始劑 75 5.2.2 光敏氟化醯酯壓克力(photosensitive fluoroimide acrylate, PSFIA)的合成 75 5.2.3 製備透過3-(三甲氧基矽基)丙基甲基丙烯酸酯(3-(trimethoxysilyl)propyl methacrylate, MPS)表面改質的膠體二氧化矽 77 5.2.3.1 改質 MA-ST-M二氧化矽 77 5.2.4 製備奈米複合材料前趨物溶液 77 5.2.5 製備奈米複合材料樣品 79 5.2.6 以熱聚合方式製備光敏氟化醯酯壓克力(thermal cured photosensitive fluoroimide acrylate, T-PSFIA)樣品 79 5.2.7 性質分析 80 5.2.7.1 傅氏轉換紅外線光譜(FT-IR) 80 5.2.7.2 核磁共振(NMR) 80 5.2.7.3 熱重量分析(TGA) 80 5.2.7.4 熱機械分析(TMA) 80 5.2.7.5 稜鏡偶合儀(Prism Coupler) 81 5.2.7.6 紫外線/可見光光譜 81 5.2.7.7 奈米硬度(Nano-indentation) 81 5.2.7.8 穿透式電子顯微鏡(TEM) 82 5.2.7.9 吸濕性行為 82 5.2.7.10 水氣滲透性行為 82 5.2.7.11 接觸角(Contact angle) 83 5.2.7.12 百格刀測試 83 5.2.8 光敏氟化醯酯壓克力的結構鑑定 83 5.2.8.1 光敏氟化醯酯壓克力(photosensitive fluoroimide acrylate, PSFIA)的結構鑑定 83 5.3 結果與討論 88 5.4 結論 102 參考文獻 103 圖目錄 Figure 2.1 Illustration of the range of domain sizes in hybrid materials[Loy, 1995]. 5 Figure 3.1 Filler volume fraction dependence for the conductivity of conductor-insulator composite [Youngs, 2002]. 11 Figure 3.2 Site percolation on the square lattice, illustrating various cluster sizes (s) for three values of p, the fraction of filled sites [Brinker, 1990]. 14 Figure 3.3 Variation of effective ε of the percolative composite, with increasing volume fraction of silver [Devaraju, 2006]. 15 Figure 3.4 Variation with silica concentration of the storage modulus at strain amplitudes < 0.1% (stars; left ordinate scale) and of the scaling exponent (right ordinate scale; squares calculated using the specific volume of the compound and circles using V corrected for the PVAc content). The vertical dashed line denotes the minimum filler concentration for formation on a silica network [Bogoslovov, 2008]. 16 Figure 3.5 Electrical conductivity of PMMA/ITO nanocomposites as a function of ITO content[Capozzi, 2008]. 16 Figure 3.6 Conductivity of the nanocomposite verse PPy content [Tang, 2009]. 17 Figure 3.7 Composite conductivity normalized to that of the bulk fillers as fuctions of volume fraction of fillers [Untereker, 2009]. 18 Figure 3.8 Electrical conductivity of aluminium-PE composites [Huang, 2009]. 18 Figure 3.9 Knoop hardness results for annealed PS-ND nanocomposite coatings as compared to the Halpin-Tsai model. The deviation from the model predictions begins ~ 13 vol% PDMS-SiOx, which supports the TEM-approximated percolation threshold[Harton, 2010]. 19 Figure 3.10 The tensile strength of EPDM composites with Si69 modified nano-zinc oxide, the dashed line in the Figures indicate the percolation point [Wang, 2010]. 19 Figure 3.11 AFM tapping mode images of samples: (a) FS-0, (b) FS-10, (c) FS-20, (d) FS-40, (e) FS-50, (f) FS-60 and (g) the phase image of FS-20. (scan size 1 μm × 1 μm, surface roughness scale in nm). 29 Figure 3.12 The processed AFM images of FS series samples. Black area indicates the nanoparticles filling area and white area is assumed as the vacancy region. Possible percolation occurs after the nanoparticle content achieves a critical value for this network. (scan size 1μm × 1μm). 30 Figure 3.13 The measured hardness linear fit as a function of SiO2 volume concentration. 31 Figure 3.14 The measured Young’s modulus linear fit as a function of SiO2 volume 31 Figure 3.15 Coefficient of thermal expansion linear fit as a function of SiO2 volume concentration. 32 Figure 3.16 Decomposition temperature linear fit as a function of SiO2 volume concentration. 32 Figure 3.17 Refractive index linear fit as a function of SiO2 volume concentration at 633 nm, 1316 nm and 1548 nm. 33 Figure 3.18 Surface morphology of FS-60 at various temperatures. (scan size 1 μm × 1 μm). 34 Figure 3.19 Thermal evolution of the area fraction of FS-60. The solid lines are obtained by Linear-Fit method. 35 Figure 4.1 IR spectra of (a) neat silica and (b) silica modified with TMES from 500 cm-1 to 4000 cm-1. 49 Figure 4.2 Effect of chemical composition on the hardness of SiO2/polymer nanocomposite, MPS- SiO2 / TEGDA-EOBDA (□) and TMES- SiO2 / PVB (○). 55 Figure 4.3 Effect of chemical compositions on the Young’s modulus of SiO2/polymer nanocomposite, MPS-SiO2 / TEGDA-EOBDA (□) and TMES-SiO2 / PVB (○). 55 Figure 4.4 Comparison of hardness of nanocomposites at different particle sizes between neat and surface-modified silica nanoparticles 59 Figure 4.5 Effect of silica content on the hardness of PVB with silica at different different particle sizes of 10, 20, 50, 100, 200 and 350 nm. 60 Figure 4.6 Effect of silica content on the Young’s modulus of PVB with silica at different different particle sizes of 10, 20, 50, 100, 200 and 350 nm. 61 Figure 4.7 Comparison of Young’s modulus of nanocomposites at different particle sizes between neat and surface-modified silica nanoparticles. 62 Figure 4.8 The FE-SEM micrographs obtain from the surface of the nanocomposites show the presence of 40 wt% SiO2 particles embedded in the PVB matrix. (a) PVB mixed with 10 nm surface-modifed SiO2 particles, (b) PVB mixed with 20 nm surface-modifed SiO2 particles, (c) PVB mixed with 50 nm surface-modifed SiO2 particles, (d) PVB mixed with 100 nm surface-modifed SiO2 particles, (e) PVB mixed with 10 nm neat SiO2 particles, (f) PVB mixed with 20 nm neat SiO2 particles, (g) PVB mixed with 50 nm neat SiO2 particles, (d) PVB mixed with 100 nm neat SiO2 particles. 64 Figure 4.9 Comparison of experimental and calculated Young’s modulus of WS series nanocomposites at different particle sizes. 65 Figure 4.10 Comparison of experimental and calculated Young’s modulus of VS series nanocomposites at different particle sizes. 66 Figure 4.11 Comparison of the hardness among chemical bonding, hydrogen bonding and Van der Waals force of nanocomposites at 20 nm silica. 68 Figure 4.12 Comparison of the Young’s modulus among chemical bonding, hydrogen bonding and Van der Waals force of nanocomposites at 20 nm silica. 68 Figure 5.1 IR spectra of (a) fluoroimide dianhydride (FIDA) and (b) fluoroimide acrylate (PSFIA) from 400 cm-1 to 4000 cm-1. 84 Figure 5.2 1H-NMR spectrum of fluoroimide dianhydride (FIDA) oligomer. 85 Figure 5.3 1H-NMR spectrum of fluoroimide acrylate (PSFIA) prepolymer. 86 Figure 5.4 Transmittance of nanocomposite films, (a) NES series and (b) NPS series. 91 Figure 5.5 TEM images of nanocomposites: (a) NES20, (b) NES40, (c) NES60, (d) NPS20, (e) NPS40 and (f) NPS60. 92 Figure 5.6 Refractive index of film samples of NES series and NPS series nanocomposites. 94 Figure 5.7 Comparison of microhardness between NES and NPS series nanocomposites. 95 Figure 5.8 Comparison of Young’s modulus between NES and NPS series nanocomposites. 95 Figure 5.9 Comparison of decomposition temperature between NES series and NPS series nanocomposites. 96 Figure 5.10 Comparison of coefficients of thermal expansion between NES series and NPS series nanocomposites. 97 Figure 5.11 Contact angles of NES series and NPS series nanocomposites. 98 Figure 5.12 (a) Comparison of contact angles between NES and NPS series, (b) water droplets on the surface of highly transparent NPS60 coated on glass and the inset shows the contact angle of the film is 142o. SEM images of nanocomposites (c) NES60 and (d) NPS60. 99 Figure 5.13 Comparison of water absorption between NES series and NPS series nanocomposites. 101 Figure 5.14 Comparison of water vapor permeation between NES series and NPS series nanocomposites. 101 表目錄 Table 2.1 Mechanical property of nylon 6-clay composites [Kojima, 1993] 7 Table 3.1 Compositions of SiO2-polyacrylate nanocomposites in weight %* 20 Table 3.2 Tg comparison of FS series (DSC, TMA and AFM) 31 Table 4.1 Compositions of modified silica nanoparticles 39 Table 4.2 Compositions of synthesized silica nanoparticles 40 Table 4.3 Compositions of SiO2 / polyacrylate nanocomposites in weight %* 41 Table 4.4 Compositions of SiO2 / PVB nanocomposites in weight % 42 Table 4.5 Compositions of modified SiO2 / PVB nanocomposites in weight % 43 Table 4.6 Particle size relationship between number of particle and total surface area at 1 g of nanoparticle. 53 Table 5.1 Compositions and acrylate functionality of T-PSFIA, NES series and NPS series of resin system. 74 Table 5.2 Prediction of fluoroimide dianhydride (FIDA) oligomer structure from proton numbers of 4,4'-(Hexafluoroisopropylidene) diphthalic anhydride (6FDA) and 4,4'-(Hexafluoroisopropylidene) dianiline (6FpDA) monomer units. 81 Table 5.3 Prediction of fluoroimide acrylate (PSFIA) prepolymer (ABA) from proton numbers of 4,4'-(Hexafluoroisopropylidene) diphthalic anhydride (6FDA) and 2-hydroxyethyl methacrylate (HEMA) monomer units. 83 Table 5.4 The adhesive properties of NES and NPS series evaluating by crosshatch adhesion test on glass substrate. 86 | |
| dc.language.iso | zh-TW | |
| dc.subject | 聚乙醯縮丁醛 | zh_TW |
| dc.subject | 有機/無機奈米複合材料 | zh_TW |
| dc.subject | 可變溫式原子力顯微鏡 | zh_TW |
| dc.subject | 透路限度 | zh_TW |
| dc.subject | 二氧化矽 | zh_TW |
| dc.subject | 氟化醯酯壓克力 | zh_TW |
| dc.subject | 透濕性 | zh_TW |
| dc.subject | 接觸角 | zh_TW |
| dc.subject | 壓克力 | zh_TW |
| dc.subject | organic/inorganic nanocomposites | en |
| dc.subject | PVB | en |
| dc.subject | acrylate and poly(vinyl butyral) | en |
| dc.subject | contact angle | en |
| dc.subject | water vapor permeation | en |
| dc.subject | fluoroimide acrylate | en |
| dc.subject | silica | en |
| dc.subject | percolation threshold | en |
| dc.subject | thermal AFM | en |
| dc.title | 有機-無機奈米複材的物性及化性研究 | zh_TW |
| dc.title | Investigation on physical and chemical properties of organic-inorganic nanocomposites | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 98-2 | |
| dc.description.degree | 博士 | |
| dc.contributor.oralexamcommittee | 邱文英(Wen-Yen Chiu),趙基揚(Chi-Yang Chao),鄭國忠(KUO-CHUNG CHENG),林更青(Keng-Ching Lin) | |
| dc.subject.keyword | 有機/無機奈米複合材料,可變溫式原子力顯微鏡,透路限度,二氧化矽,氟化醯酯壓克力,透濕性,接觸角,壓克力,聚乙醯縮丁醛, | zh_TW |
| dc.subject.keyword | organic/inorganic nanocomposites,thermal AFM,percolation threshold,silica,fluoroimide acrylate,water vapor permeation,contact angle,acrylate and poly(vinyl butyral),PVB, | en |
| dc.relation.page | 116 | |
| dc.rights.note | 未授權 | |
| dc.date.accepted | 2010-08-16 | |
| 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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