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論文名稱 Title |
團狀共聚物作模板合成可調控中孔洞材料:形態,相行為及應用 Morphology, Phase behavior and Application of Tunable Mesoporous Materials Templated by Block copolymers. |
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系所名稱 Department |
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畢業學年期 Year, semester |
語文別 Language |
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學位類別 Degree |
頁數 Number of pages |
272 |
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研究生 Author |
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指導教授 Advisor |
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召集委員 Convenor |
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口試委員 Advisory Committee |
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口試日期 Date of Exam |
2013-01-04 |
繳交日期 Date of Submission |
2013-01-22 |
關鍵字 Keywords |
中孔洞二氧化矽、嵌段共聚物、酚醛樹脂、揮發誘導自組裝 Evaporation Induced Self-assembly (EISA), block copolymer, mesoporous silica, phenolic resin |
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統計 Statistics |
本論文已被瀏覽 5739 次,被下載 202 次 The thesis/dissertation has been browsed 5739 times, has been downloaded 202 times. |
中文摘要 |
本論文,我們利用了數種獨特的兩性嵌段共聚物如 PE-PEO、 PEO-PCL、 PEO-PLLA、PE-PEO-PLLA 及 PE-PEO-PCL 等作為模板,並透過揮發導致自組裝 方法去合成一系列的中孔洞二氧化矽、中孔洞酚醛樹脂及中孔洞碳材等中孔洞材 料。 首先,我們使用 PE-PEO 作為樣板,去研究 TOES 與模板以及鹽酸及模板重 量比在揮發導致自組裝過程中的影響,並以熱力學及動力學的觀念去解析之。另 外,我們延伸這個研究方法至其他的嵌段共聚物模板系統,特別是 ABC 三嵌段共 聚物作為單一模板這個系統,可得到多層次結構的中孔洞材料。此外,我們使用 開環聚合方法去合成一系列的嵌段共聚物模板,此合成方法使嵌段共聚物模板的 可變性更為增加,藉此可調控所合成的中孔洞材料孔徑或形貌的不同。另外混摻 技巧也可應用在合成中孔洞材料的揮發導致自組裝過程中,更可輕易的調控中孔 洞材料的樣貌或孔徑等性質,最後我們將中孔洞材料薄膜應用在易揮發有機化合 物的蒸氣偵測上,由於中孔洞材料高比表面積的特性,因此在偵測的表現上有很 好的效果。 |
Abstract |
In the study, we have utilized several unique amphiphilic block copolymers as templates, such as PE-PEO, PEO-PCL, PEO-PLLA, PE-PEO-PLLA and PE-PEO-PCL, to successfully fabricate a series of mesoporous materials, for example, mesoporous silicas, mesoporous phenolic resins and mesoporous carbons by a convenient EISA method. Firstly, we took PE-PEO as model block copolymer to study the TEOS-to-template or HCl-to-template weight ratio effect during the EISA process, view from the thermal dynamic point and kinetic reason, respectively. In addition, we expended the research method to the other block copolymer systems, especially for the unusual ABC type triblock copolymers, we obtained the hierarchical mesostructure by single template. Furthermore, the lab-made amphiphilc block copolymer that synthesized from ring-opening polymerization (ROP) could increase the possibility of the mesoporous materials field by tuning the segment length through synthesis technique. Moreover, blending technique could also be used in the templating process during EISA, the clear method could easily control the morphology and pore size of the mesoporous materials. Eventually we take our mesoporous thin film as the volatile organic compounds (VOCs) sensors and obtain great results due to the large surface area of the mesoporous materials. |
目次 Table of Contents |
Content 摘要 ................................................................................................................................ i Abstract .......................................................................................................................... ii Content ......................................................................................................................... iii Table Captions .............................................................................................................. ix Figure Captions ............................................................................................................ xi Chapter 1 introduction ................................................................................................... 1 1-1 Mesoporous materials ........................................................................................ 1 1-2 Evaporation-induced self-assembly (EISA) ....................................................... 3 1-3 Block copolymers ............................................................................................... 5 1-4 Motivation ........................................................................................................... 8 1-5 References ........................................................................................................ 10 Chapter 2 Phase Behavior of Mesoporous Silicas Templated by the Amphiphilic Diblock Copolymer Poly(ethylene-b-ethylene oxide) ................................................. 13 2-1 Background: .................................................................................................. 13 2-2 Experimental: ................................................................................................ 16 2-2-1Materials ........................................................................................ 16 2-2-2 Synthesis of the mesoporous silica ................................................ 16 2-2-2 Characterization ........................................................................... 17 2-3 Results and disscussion .................................................................................... 19 2-3-1 Mesoporous silica samples synthesized at various TEOS–to–PE-b-PEO ratios .................................................................... 19 2-3-2 Mesoporous silica samples synthesized at different HCl–to–PE-b-PEO weight fractions ...................................................... 25 2-4 Summary .......................................................................................................... 31 Chapter 3 Tunable Mesoporous Lamellar Silicas Prepared Using Poly(ethylene oxide-b-l-lactide) and Poly(ethylene-b-ethylene oxide-b-l-lactide) Block Copolymers as Templates ..................................................................................................................... 36 3-1 Background: .................................................................................................. 36 3-2 Experimental: ................................................................................................ 38 3-2-1Materials ........................................................................................ 38 3-2-2 PEO-PLLA and PE-PEO-PLLA Block Copolymers ..................... 38 3-2-3 Mesoporous silicas synthesized using PEO-PLLA diblock copolymers and PE-PEO-PLLA triblock terpolymers as templates ....... 39 3-2-4 Characterization ........................................................................... 39 3-3 Results and disscussion .................................................................................... 41 3-3-1 Characterization of mesoporous silicas prepared using PEO-PLLA diblock copolymers as templates ............................................................ 41 3-3-1 Characterization of mesoporous silicas prepared using PE-PEO-PLLA triblock copolymers as templates .................................. 53 3-4 Summary .......................................................................................................... 63 3-5 References ........................................................................................................ 64 Chapter 4 Phase Behavior of Hierarchical Mesoporous Silicas Prepared Using ABC Triblock Copolymers as Single Templates .................................................................. 66 4-1 Background: .................................................................................................. 66 4-2 Experimental: ................................................................................................ 69 4-2-1 Materials ....................................................................................... 69 4-2-2 PE-PEO-PCL copolymers of various molecular weights ............. 69 4-2-3 Mesoporous silicas templated by PE-PEO-PCL copolymers ....... 69 4-2-4 Characterization ........................................................................... 70 4-3 Results and disscussion .................................................................................... 72 4-3-1 Characterization of PE-PEO-PCL copolymers ............................ 72 4-3-2 Mesoporous silicas prepared using E 13 EO 42 CL 31 as template; tetragonal cylinder in FCC hierarchical nanostructure ......................... 75 4-3-3 Mesoporous silicas prepared using E 13 EO 42 CL 9 as template; simple cubic in BCC hierarchical nanostructure ................................... 78 4-3-4 Mesoporous silicas templated by various PE-PEO-PCL copolymers at different TEOS–to– PE-PEO-PCL weight ratios ............ 83 4-3-5 Mesoporous silicas templated by E 13 EO 42 CL 31 copolymers at various HCl (aq) contents .......................................................................... 92 4-3-6 Mesoporous silicas templated by different PE-PEO-PCL copolymers at a constant TEOS-to-template weight ratio ..................... 95 4-4 Summary .......................................................................................................... 99 4-5 References ...................................................................................................... 100 Chapter 5 Templating Amphiphilic Poly(ethylene oxide-b-ε-caprolactone) Diblock Copolymers Provide Ordered Mesoporous Silicas with Large Tunable Pores ......... 102 5-1 Background: ................................................................................................ 102 5-2 Experimental: .............................................................................................. 104 5-2-1 Materials ..................................................................................... 104 5-2-1 Synthesis of mesoporous silicas templated by PEO-b-PCL copolymers of various molecular weights ............................................ 105 5-2-3 Synthesis of mesoporous silicas templated by PEO-b-PCL copolymers blended with homopolymer additives ................................ 105 5-2-4 Characterization ......................................................................... 106 5-3 Results and disscussion .................................................................................. 108 5-3-1 Body-centered cubic mesoporous silica templated by amphiphilic block copolymer EO 114 CL 20 .................................................................. 108 5-3-2 Mesoporous silicas templated by PEO-b-PCL copolymers with PCL blocks of different molecular weights ............................................ 111 5-3-3 Mesoporous silicas prepared using PCL homopolymers as pore expander from EISA ............................................................................... 115 5-3-4 Mesoporous silicas prepared using PEO-POSS and PEO as modifiers for EISA ................................................................................ 121 5-4 Summary ........................................................................................................ 125 5-5 References ...................................................................................................... 126 Chapter 6 From Microphase Separation to Self-Organized Mesoporous Phenolic Resin through Competitive Hydrogen Bonding with Double-Crystalline Diblock Copolymers of Poly(ethylene oxide-b-ε-caprolactone) ................................................................. 127 6-1 Background: ................................................................................................ 127 6-2 Experimental: .............................................................................................. 129 6-2-1 Materials. .................................................................................... 129 6-2-1 Synthesis of mesoporous phenolic resins and carbon ................. 130 6-2-1 Characterizations. ....................................................................... 131 6-3 Results and disscussion .................................................................................. 133 6-3-1 Phenolic Resin/Block Copolymer Analyses ................................ 133 6-3-2 Mesoporous Phenolic Resin Analyses ......................................... 144 6-3-3 SAXS, TEM and BET Analyses of Mesoporous Phenolic Resin .. 147 6-3-4Morphology of mesoporous carbon ............................................. 159 6-4 Summary ........................................................................................................ 162 6-5 References ...................................................................................................... 163 Chapter 7 Transformations and Enhanced Long-Range Ordering of Mesoporous Phenolic Resin Templated by Poly(ethylene oxide-b-ε-caprolactone) Block Copolymers Blended With Star Poly(ethylene oxide)–Functionalized Silsesquioxane (POSS) ... 166 7-1 Background: ................................................................................................ 166 7-2 Experimental: .............................................................................................. 169 7-2-1 Materials ..................................................................................... 169 7-2-2 Synthesis of mesoporous phenolic resins .................................... 170 7-2-3 Characterization ......................................................................... 170 7-3 Results and disscussion .................................................................................. 172 7-3-1 Synthesis of mesoporous phenolic resins templated by PEO-b-PCL copolymer ............................................................................................. 172 7-3-2 DSC and FTIR spectroscopic analyses of phenolic/PEO-b-PCL/PEO-POSS ternary blends ................................ 174 7-3-3 Synthesis of mesoporous phenolic resins templated by PEO-b-PCL/PEO-POSS blends ........................................................... 178 7-3-4 Synthesis and morphology of mesoporous carbon ...................... 194 7-4 Summary ........................................................................................................ 198 7-5 References ...................................................................................................... 199 Chapter 8 Mesoporous Nanostructures Templated by Amphiphilic Crystalline–Crystalline Diblock Copolymers of Poly(ethylene oxide-b-ε-caprolactone) and applying to Sense Volatile Organic Compound .................................................. 202 8-1 Background: ................................................................................................ 202 8-2 Experimental: .............................................................................................. 206 8-2-1 Materials ..................................................................................... 206 8-2-2 Synthesis of PEO-b-PCL Block Copolymer ................................ 206 8-2-3 Synthesis of the Mesoporous Silicas ........................................... 207 8-2-4 Synthesis of mesoporous phenolic resins .................................... 207 8-2-5 Characterization ......................................................................... 208 8-2-6 Preparation of VOCs sensor ....................................................... 210 8-2-7 Sensing Experiment for VOCs..................................................... 210 8-3 Results and disscussion .................................................................................. 212 8-3-1 Synthesis of PEO-b-PCL ............................................................. 212 8-3-2 Phase behavior of mesoporous silicas ........................................ 215 8-3-3 Phase behavior of mesoporous phenolic resins .......................... 223 8-3-4 Mesoporous thin films for VOCs sensing .................................... 233 8-4 Summary ........................................................................................................ 237 8-5 References ...................................................................................................... 238 Chapter 9 Conclusions ............................................................................................... 241 Resume ...................................................................................................................... 244 Table Captions Table 1-1. Classification of pore size……………………………………………………2 Table 1-2. Famous mesoporous materials and their mesostructure……………………..2 Table 2-1. Textual properties of the mesoporous silicas. ………………………………30 Table 3-1: Characterization of PEO-PLLA & PE- PEO-PLLA block copolymers used in this study………………………………………………………………………………51 Table 3-2. Textual properties of various mesoporous silica samples………………….52 Table 4-1: Characterization data of PE-PEO-PCL triblock copolymers used in this study……………………………………………………………………………………75 Table 4-2. Textural properties of the hierarchical mesoporous silica (“simple cubic in BCC”, sample E1T40) …………………………………………………………………83 Table 4-3. Textural properties of mesoporous silica samples templated by PE-PEO-PCL at various TEOS–to–PE-PEO-PCL ratios………………………………………………93 Table 4-4: Textural properties of mesoporous silica samples templated by PE-PEO-PCL at various TEOS–to–PE-PEO-PCL–to–HCl (aq) weight fractions. …………………..…97 Table 4-5: Textural properties of mesoporous silica samples templated by PE-PEO-PCL with various PCL molecular weights at the same TEOS–to–PE-PEO-PCL ratio…….100 Table 5-1: Characterization of PEO-b-PCL diblock copolymers used in this study…………………………………………………………………………….……..108 Table 5-2. Textural properties of mesoporous silicas templated by different block copolymers and homopolymers…………………………………………………...…..118 Table 6-1: Characterization of PCL-b-PEO-b-PCL triblock copolymer and PEO-b-PCL diblock copolymers used in this study……………………………………………...…140 Table 6-2: Thermal properties of Phenolic/EC blends…………………………...…...144 Table 6-3: Summary of the self-association and inter-association equilibrium constants and thermodynamic parameter of phenolic/EC blends at room temperature…………150 Table 6-4. Textual properties of the mesoporousphenolic resins and carbon products.164 Table 7-1: Characterization of PEO-b-PCL diblock copolymers used in this study….175 Table 7-2. Textural properties of the mesoporous phenolic resin structures……….…193 Table 7-3. Textual properties of the mesoporous carbon……………………………...203 Table 8-1. Textual properties of the mesoporous silicas, phenolic resins and carbon products……………………………………………………………………………….228 Table 8-2: Curve-fitting result of phenolic/PEO-b-PCL blend at room temperature…236 Figure Captions Figure 1-1. The well-known structure of mesoporous materials. ……………………….2 Figure 1-2. Evaporation induced self-assembly (EISA) ………………………………...4 Figure 1-3. Factors affected morphologies of mesomaterials and their relationship during EISA. …………………………………………………………………………….4 Figure 1-4. Phase diagram of block copolymer microphase separation. ………………..7 Figure 2-1. SAXS patterns of mesoporous silica samples prepared at various TEOS–to–PE-b-PEO weight ratios…………………………………………………….22 Figure 2-2. TEM images of mesoporous silica samples prepared at TEOS–to–PE-b-PEO weight ratios of (a) 3.4:1, (b) 5.6:1, (c) 10:1, and (d) 11:1…………………………….23 Figure 2-3. TEM images of microtomed mesoporous silica samples prepared at a TEOS–to–PE-b-PEO weight ratio of 5.6:1. (a) Top view; (b) side view of hexagonal cylinders. ………………………………………………………………………………24 Figure 2-4. (A) N 2 adsorption/desorption isotherms and (B) pore size distribution curves of mesoporous silica samples prepared at various TEOS–to–PE-b-PEO weight ratios……………………………………………………………………………………24 Figure 2-5. SAXS patterns of mesoporous silica samples templated by PE-b-PEO at various HCl–to–PE-b-PEO weight fractions…………………………………………..27 Figure 2-6. TEM images of mesoporous silica samples templated by PE-b-PEO at HCl–to–PE-b-PEO weight ratios of (a) 0.80, (b) 0.16, (c) 0.12, and (d) 0.06…………28 Figure 2-7. TEM images of microtomed mesoporous silica samples templated by PE-b-PEO at a HCl–to–PE-b-PEO weight ratio of 0.12. (a) Hexagonal cylindrical mesopores; (b) spherical mesopores with b.c.c. packing………………………………29 Figure 2-8. (A) N 2 adsorption/desorption isotherms and (B) pore size distribution curves of mesoporous silica samples templated by PE-b-PEO at various HCl–to–PE-b-PEO weight ratios……………………………………………………………………………29 Figure 3-1. GPC traces of (a) the homopolymer PEO 114 (black line) and (b, c) the diblock copolymers (b) EO 114 LLA 26 (red dashed line) and (c) EO 114 LLA 130 (blue dashed line)…………………………………………………………………………………….44 Figure 3-2. 1 H NMR spectra of the PEO-PLLA copolymers (in CDCl 3 ) (a) EO 114 LLA 26 and (b) EO 114 LLA 130 ……………………………………………………………………45 Figure 3-3. SAXS patterns of the mesoporous silicas templated by EO 114 LLA 26 at various TEOS–to–EO 114 LLA 26 weight ratios…………………………………………..46 Figure 3-4. TEM images of mesoporous silicas templated by EO 114 LLA 26 , prepared at TEOS-to-EO 114 LLA 26 weight ratios of (a) 1:1, (b) 2:1, (c) 3:1, (d) 5:1, (e) 10:1 and (f) 15:1……………………………………………………………………………………..47 Figure 3-5. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by EO 114 LLA 26 at various TEOS–to–EO 114 LLA 26 weight ratios……………………………………………………………………………48 Figure 3-6. SAXS patterns of mesoporous silicas templated by EO 114 LLA 26 at various TEOS–to–EO 114 LLA 130 weight ratios………………………………………………….49 Figure 3-7. TEM images of mesoporous silicas templated by EO 114 LLA 26 at TEOS–to–EO 114 LLA 130 weight ratios of (a) 1:1, (b) 3:1, (c) 5:1, (d) 10:1, and (e) 15:1. Figure 3-8. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by EO 114 LLA 130 at various TEOS–to–EO 114 LLA 130 weight ratios……………………………………………………………………………50 Figure 3-9. GPC traces of (a) the diblock copolymer E 13 EO 42 (black line) and (b, c) the triblock terpolymers (b) E 13 EO 42 LLA 26 (red dashed line) and (c) E 13 EO 42 LLA 35 (blue dashed line)……………………………………………………….……………………56 Figure 3-10. 1 H NMR spectra of the PE-PEO-PLLA copolymers (in CDCl 3 ) (a) E 13 EO 42 LLA 26 and (b) E 13 EO 42 LLA 35 …………………………………………………57 Figure 3-11. SAXS patterns of mesoporous silicas templated by E 13 EO 42 LLA 26 at various TEOS–to–E 13 EO 42 LLA 26 weight ratios………………………………………..58 Figure 3-12. TEM images of mesoporous silicas templated by E 13 EO 42 LLA 26 , prepared at TEOS-to-EO 114 LLA 26 weight ratios of (a) 1:1, (b) 2:1, (c) 3:1, (d) 3.5:1, (e) 4:1 and (f) 5:1………………………………………………………………………………………59 Figure 3-13. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by E 13 EO 42 LLA 26 at various TEOS–to–E 13 EO 42 LLA 26 weight ratios……………………………………………………………………………60 Figure 3-14. SAXS patterns of mesoporous silicas templated by E 13 EO 42 LLA 35 at various TEOS–to–E 13 EO 42 LLA 35 weight ratios………………………………………..61 Figure 3-15. TEM images of mesoporous silicas templated by E 13 EO 42 LLA 35 with different TEOS-to-E 13 EO 42 LLA 35 weight ratio. ………………………………………62 Figure 3-16. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by E 13 EO 42 LLA 35 at various TEOS–to–E 13 EO 42 LLA 35 weight ratios……………………………………………………………………………62 Figure 4-1. GPC traces of the diblock copolymer E 13 EO 42 (black line) and the triblock copolymers E 13 EO 42 CL 9 (red dashed line), E 13 EO 42 CL 18 (blue dashed line), E 13 EO 42 CL 31 (magenta dashed line), and E 13 EO 42 CL 44 (green dashed line)…………...74 Figure 4-2. 1 H NMR spectra of the copolymers PE-PEO and PE-PEO-PCL in CDCl 3 ..75 Figure 4-3. SAXS pattern (a) and microtomed TEM images of mesoporous silicas templated by PE 13 -b-PEO 42 -b-PCL 31 viewed from [001] (b), [10] (c), and [11] (d) directions. Insets are corresponding FFT diffractograms. (e) N 2 adsorption-desorption isotherms and (f) pore size distribution curves of mesoporous silicas templated by PE 13 -b-PEO 42 -b-PCL 31 …………………………………………………………………78 Figure 4-4. (a) SAXS pattern, (b) 3D model of “simple cubic in BCC” hierarchical structure and viewed from the (c) [100], (d) [110], and (e) [111] planes of the “simple cubic in BCC” mesoporous silica templated by E 13 EO 42 CL 9 at a TEOS-to- E 13 EO 42 CL 9 ratio of 4:1……………………………………………………………………………...81 Figure 4-5. TEM images (4a-c), corresponding FFT (4d-f) and the foreseeable diagrams (4g-i) of the “simple cubic in BCC” mesoporous silica viewed from the [100] (4a, 4d and 4g), [110] (4b, 4e and 4h), and [111] (4c, 4f and 4i) planes, respectively…………82 Figure 4-6. (a) N 2 adsorption/desorption isotherm, and (b) pore size distribution curve of the “simple cubic in BCC” mesoporous silica templated by E 13 EO 42 CL 9 at a TEOS-to- E 13 EO 42 CL 9 ratio of 4:1……………………………………………………..83 Figure 4-7. (a) TEM images, (b) SAXS patterns, (c) N 2 adsorption/desorption isotherms, and (d) pore size distribution curves of mesoporous silicas templated by E 13 EO 42 CL 9 at TEOS-to-E 13 EO 42 CL 9 weight fractions of 2.5:1, 3.0:1, 3.5:1, 4:1, and 4.5:1………….89 Figure 4-8. (a) TEM images, (b) SAXS patterns, (c) N 2 adsorption/desorption isotherms, and (d) pore size distribution curves of mesoporous silicas templated by E 13 EO 42 CL 18 at TEOS-to-E 13 EO 42 CL 18 weight fractions of 2.5:1, 3.0:1, 3.5:1, 4:1, and 4.5:1…………90 Figure 4-9. (a) TEM images, (b) SAXS patterns, (c) N 2 adsorption/desorption isotherms, and (d) pore size distribution curves of mesoporous silicas templated by E 13 EO 42 CL 31 at TEOS-to-E 13 EO 42 CL 31 weight fractions of 2.5:1, 3.0:1, 3.5:1, 4:1, and 4.5:1…………91 Figure 4-10. (a) TEM images, (b) SAXS patterns, (c) N 2 adsorption/desorption isotherms, and (d) pore size distribution curves of mesoporous silicas templated by E 13 EO 42 CL 44 at TEOS-to-E 13 EO 42 CL 44 weight fractions of 2.5:1, 3.0:1, 3.5:1, 4:1, and 4.5:1……………………………………………………………………………………92 Figure 4-11. (a) TEM images, (b) SAXS patterns, (c) N 2 adsorption/desorption isotherms, and (d) pore size distribution curves of mesoporous silicas templated by E 13 EO 42 CL 31 at TEOS-to-E 13 EO 42 CL 31 -to-HCl (aq) weight fractions of 3.5:1:0.5, 3.5:1:1.0, 3.5:1:1.5, and 3.5:1:2.0……………………………………………………..96 Figure 4-12. (a) TEM images, (b) SAXS patterns, (c) N 2 adsorption/desorption isotherms, and (d) pore size distribution curves of mesoporous silicas templated by various PE-PEO-PCL copolymers at a TEOS-to-EO 114 CL 20 weight fraction of 3.5:1…99 Figure 5-1. (a) SAXS pattern, (b–d) TEM images viewed from [100], [110], and [111], respectively (insets: corresponding FFT), (e) N 2 adsorption/desorption isotherm, and (f) pore size distribution curve of bcc mesoporous silica templated by EO 114 CL 20 with a TEOS/EO 114 CL 20 ratio of 2:1…………………………………………………………114 Figure 5-2. (a) SAXS patterns and (b–e) TEM images of mesoporous silicas templated by EO 114 CL n at weight fractions of (b) TEOS/EO 114 CL 20 = 2:1, (c) TEOS/EO 114 CL 42 = 3:1, (d) TEOS/EO 114 CL 84 = 5:1, and (e) TEOS/EO 114 CL 130 = 11:1…………………...117 Figure 5-3. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by EO 114 CL n at TEOS/EO 114 CL n weight fractions of 2:1 (n = 20), 3:1 (n = 42), 5:1 (n = 84), and 11:1 (n = 130)…………………………...117 Figure 5-4. (a) SAXS patterns and (b–e) TEM images of mesoporous silicas templated by EO 114 CL 20 at TEOS/EO 114 CL 20 /PCL 20 weight fractions of (b) 2:1:0, (c) 2:1:0.1, (d) 2:1:0.3, and (e) 2:1:0.5………………………………………………………………..123 Figure 5-5. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by EO 114 CL 20 at TEOS/EO 114 CL 20 /PCL 20 weight fractions of 2:1:0, 2:1:0.1, 2:1:0.3, and 2:1:0.5……………………………………….123 Figure 5-6. (a) SAXS patterns and (b–e) TEM images of mesoporous silicas templated by EO 114 CL 20 at TEOS/EO 114 CL 20 /PCL 408 weight fractions of (b) 2:1:0, (c) 2:1:0.1, (d) 2:1:0.3, and (e) 2:1:0.5………………………………………………………………..124 xvi Figure 5-7. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by EO 114 CL 20 at TEOS/EO 114 CL 20 /PCL 408 weight fractions of 2:1:0, 2:1:0.1, 2:1:0.3, and 2:1:0.5……………………………………….124 Figure 5-8. (a) SAXS patterns and (b–e) TEM images of mesoporous silicas templated by EO 114 CL 84 at TEOS/EO 114 CL 84 /PCL 20 weight fractions of (b) 3:1:0, (c) 3:1:0.5, (d) 3:1:0.7, and (e) 3:1:0.9………………………………………………………………..125 Figure 5-9. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by EO 114 CL 84 at TEOS/EO 114 CL 84 /PCL 20 weight fractions of 3:1:0, 3:1:0.5, 3:1:0.7, and 3:1:0.9………………………………………125 Figure 5-10. (a) SAXS patterns and (b–e) TEM images of mesoporous silicas templated by EO 114 CL 84 at TEOS/EO 114 CL 84 /PEO 13 -POSS weight fractions of 3:1:0, 3:1:0.3, 3:1:0.5, and 3:1:0.7……………………………………………………………………129 Figure 5-11. (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous silicas templated by EO 114 CL 84 at TEOS/EO 114 CL 84 /PEO 13 -POSS weight fractions of 3:1:0, 3:1:0.3, 3:1:0.5, and 3:1:0.7……………………………………….129 Figure 5-12. (a) SAXS patterns and (b–e) TEM images of mesoporous silicas templated by EO 114 CL 84 at TEOS/EO 114 CL 84 /PEO 22 weight fractions of 3:1:0, 3:1:0.3, 3:1:0.5, and 3:1:0.7…………………………………………………………………………………130 Figure 6-1: DSC thermograms of phenolic/EC blends, having different compositions for (a) phenolic/EC1, (b) phenolic/EC2, (c) phenolic/EC3, and (d) phenolic/EC………..143 Figure 6-2: FT-IR spectra recorded at room temperature displaying the (a) hydroxyl stretching, (b) carbonyl, and (c) ether region…………………………………………149 Figure 6-3: FT-IR spectra recorded at room temperature displaying the carbonyl region of phenolic/EC blends fixing phenolic contents (50 and 60 wt%) for (a) pure EC1, (b) phenolic/EC1, (c) phenolic/EC2, (d) phenolic/EC3, and (e) phenolic/EC4………….150 Figure 6-4: Experimental and prediction data for of phenolic/EC blends with different phenolic weight percent for (█) phenolic/EC1, (●) phenolic/EC2, (▲) phenolic/EC3, and (▼) phenolic/EC4………………………………………………..151 Figure 6-5: DSC cooling curves of phenolic/EC blends after curing HMTA for (a) phenolic/EC1, (b) phenolic/EC2, (c) phenolic/EC3 and (d) phenolic/EC4 with a constant cooling rate of 5 °C /min…………………………………………………….155 Figure 6-6: Profiles of Lorentz-corrected SAXS intensity of mesoporous phenolic resin from templated by (a) EC1, (b) EC2, (c) EC3, and (d) EC4 block copolymers………159 Figure 6-7: TEM images of mesoporous phenolic from phenolic/EC1 for (a) 30/70, (b) 40/60, (c) 50/50, (d) 60/40, phenolic/EC2 for (e) 40/60, (f) 50/50, (g) 60/40, (h) 70/30, phenolic/EC3 for (i) 50/50, (j) 60/40, phenolic/EC4 for (k) 50/50, and (l) 60/40 blends………………………………………………………………………………….160 Figure 6-8: Summary of SAXS analyses (A) and TEM images of mesoporous phenolic resin containing fixing 50 wt% phenolic resin contents with different templated block copolymers for (B) EC1, (C) EC2, (D) EC3, and (E) EC4. ………………………….160 Figure 6-9: Phase diagram of (A) phenolic/EC blends, the open circle represent miscible disorder structure, the full circles represent microphase separation structure and (B) mesoporous phenolic resin from template by EC block copolymers, the open circles represent disorder structure and the full circles represent regular mesoporous structure. ……………………………………………………………………………..161 Figure 6-10: N 2 adsorption-desorption isotherms of mesoporous phenolic resins templated by different EC block copolymers with different phenolic weight percents (a) 50 wt%, and (b) 60 wt%................................................................................................162 Figure 6-11: pore size distribution curves of mesoporous phenolic resins templated by different EC block copolymers with different phenolic weight percents (a) 50 wt%, and (b) 60 wt%.....................................................................................................................163 Figure 6-12: SAXS pattern (a), TEM images (b), (c), and (d), N 2 adsorption-desorption isotherms (e), and pore size distribution curves (f) of mesoporous of gyroid mesoporous carbon pyrolyzed from mesoporous phenolic resin templated by EC2 block copolymer at 50 wt% phenolic resin content at 800 °C…………………………………………..167 Figure 7-1: (a) SAXS analyses and (b–g) TEM images of mesoporous phenolic resin structures containing a fixed phenolic resin content (50 wt%) and the templating block copolymers (b, c) EC1, (d, e) EC2, and (f, g) EC3……………………………………179 Figure 7-2: DSC thermograms of phenolic/EC2/PEO-POSS ternary blends at (a) 50/50/0, (b) 50/50/6, (c) 50/50/10, (d) 50/50/18, and (e) 50/50/26 ratios…………….183 Figure 7-3: FTIR spectra of phenolic/EC3/PEO-POSS systems, recorded at room temperature, displaying the (a) OH, (b) C=O, and (c) ether regions………………….184 Figure 7-4: Profiles of SAXS intensities of mesoporous phenolic resin structures obtained from templating EC1/PEO-POSS blends…………………………………...192 Figure 7-5: TEM images of mesoporous phenolic structures obtained from phenolic/EC1/PEO-POSS blends…………………………………………………….192 Figure 7-6: (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous phenolic resins templated by EC1/PEO-POSS blends………………193 Figure 7-7: Profiles of SAXS intensities of mesoporous phenolic resin structures obtained from templating EC2/PEO-POSS blends………………………………….194 Figure 7-8: TEM images of mesoporous phenolic structures obtained from phenolic/EC2/PEO-POSS blends……………………………………………………194 Figure 7-9: (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous phenolic resin structures templated by EC2/PEO-POSS blends…….195 Figure 7-10: Profiles of SAXS intensities of mesoporous phenolic resin structures obtained from templating EC3/PEO-POSS blends…………………………………..196 Figure 7-11: TEM images of mesoporous phenolic structures obtained from phenolic/EC3/PEO-POSS blends…………………………………………………….196 Figure 7-12: (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of mesoporous phenolic resin structures obtained from templating EC3/PEO-POSS blends…………………………………………………………………………………197 Figure 7-13: Phase diagram of mesoporous phenolic resin from template by EC/PEO-POSS blends, the open circles represent disorder structure, the full circles represent regular mesoporous structure templated by pure EC diblock copolymer and the hexagonal symbols represent regular mesoporous structure templated by EC/PEO-POSS blends ……………………………………………………………….199 Figure 7-14: Scale expanded phase diagram of phenolic/EC/PEO-POSS with different PEO+PEO-POSS weight fraction at phenolic resin content (ca. 0.35~0.5), the black and white symbol represents lamellae, triangle symbol represents gyroid, hexagonal symbol represents cylinder, circle symbol represents sphere mesoporous structure………….199 Figure 7-15: (a, b) TEM images of gyroid mesoporous carbon structures pyrolyzed from the phenolic/EC3 = 50/50 system. (c, d) TEM images and (e, f) field-emission SEM images of cylinder mesoporous carbon structures pyrolyzed from the phenolic/EC3/PEO-POSS = 50/50/22 system at 800 °C……………………………..202 Figure 7-16: (a) N 2 adsorption/desorption isotherms and (b) pore size distribution curves of gyroid mesoporous carbon structures pyrolyzed from the phenolic/EC3 = 50/50 system and (c) N 2 adsorption/desorption isotherms and (d) pore size distribution curves of cylinder mesoporous carbon structures pyrolyzed from the phenolic/EC3/PEO-POSS = 50/50/22 system at 800 °C…………………………………………………………203 Figure 8-1: 1 H NMR of PEO-b-PCL copolymer (in CDCl 3 )…………………………219 Figure 8-2: TGA analysis of PEO-b-PCL block copolymer under nitrogen………….220 Figure 8-3: TGA analysis of PEO-b-PCL block copolymer under air………………..220 Figure 8-4. DSC thermograms of the crystallization curve with different ratios of silica/PEO-b-PCL……………………………………………………………………..225 Figure 8-5. SAXS patterns of mesoporous silicas templated by PEO-b-PCL with different TEOS/PEO-b-PCL weight fractions………………………………………...225 Figure 8-6. TEM images of mesoporous silicas templated by PEO-b-PCL with different TEOS/PEO-b-PCL weight fractions: (a)1/1, (b)5/1, (c)10/1, and (d)15/1……………226 Figure 8-7. FE-SEM images of mesoporous silicas templated by PEO-b-PCL with different TEOS/PEO-b-PCL weight fractions: (a)1/1 and (b)5/1…………………….226 Figure 8-8. (A) N 2 adsorption-desorption isotherms and (B) pore size distribution curves of mesoporous silicas templated by PEO-b-PCL with different TEOS/PEO-b-PCL weight fractions………………………………………………………………………227 Figure 8-9. DSC thermograms of (a) second heat scan and (b) first cooling scan of phenolic/PEO-b-PCL blends, (c) first cooling scan of phenolic/PEO-b-PCL blends after curing…………………………………………………………………………………235 Figure 8-10. FT-IR spectra at room temperature of the phenolic/PEO-b-PCL blend displaying the (a) hydroxyl, (b) carbonyl and (c) ether region………………………236 Figure 8-11. SAXS patterns of mesoporous phenolic resins from different weight fractions of phenolic/PEO-b-PCL blends……………………………………………237 Figure 8-12. TEM image of mesoporous phenolic resins from different weight fractions of phenolic/PEO-b-PCL blends: (a) 40/60, (b) 50/50, (c) 60/40, and (d) 70/30……..238 Figure 8-13 . (A) N 2 adsorption-desorption isotherms and (B) pore size distribution curves of mesoporous resins templated by PEO-b-PCL with different phenolic/PEO-b-PCL weight fractions………………………….…………………….238 Figure 8-14. Performance curve of the gas sensor……………………………………241 Figure 8-15. (a) Sensitivity of mesoporous silica chips toward various VOCs, each at a concentration of 16 ppm. (b) Temporal sensitivities of mesoporous and nonporous silica sensors toward formaldehyde vapor (16 ppm)………………………………………..241 Figure 8-16. (a) Sensitivity of mesoporous phenolic resin chips toward various VOCs, each at a concentration of 16 ppm. (b) Response of the mesoporous phenolic sensor to repeated dosing with benzene vapor at 100 ppm. (c) Temporal sensitivities of mesoporous and nonporous phenolic sensors…………………………………………242 |
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