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Self-supporting Polymer from a POSS Derivative
(2011-06-16)
Cheng, Chih-Chia
;
Yen, Ying-Chieh
;
Chang, Feng-Chih
;
應用化學系
;
Department of Applied Chemistry
A new polyhedral oligomeric silsesquioxane macromer, octakis[N-(6-aminopyridin-2-yl)-undecanamide-10-dimethyl-siloxy]silsesquioxane (POSS-C11-Py), containing eight diaminopyridine arms, is able to self-assemble to form a physically crosslinked polymer-like structure with good mechanical properties (tensile strength = 46.1 MPa, tensile modulus = 0.58 GPa, elongation = 49.3%) through quadruple hydrogen bonding interactions between these arms. POSS-C11-Py is the first organic/inorganic supermolecule possessing polymer-like mechanical properties as a result of self-complementary interactions, providing a potential route toward the design and fabrication of polymer-like supramolecular materials.
Syntheses and specific interactions of poly (hydroxyethyl methacrylate-b-vinyl pyrrolidone) diblock copolymers and comparisons with their corresponding miscible blend systems
(2006-09-20)
Huang, Chih-Feng
;
Kuo, Shiao-Wei
;
Lin, Fang-Ju
;
Wang, Chih-Feng
;
Hung, Chen-Jui
Combination of atom transfer radical and conventional free radical polymerizations has been successfully used to prepare poly(hydroxyethyl methacrylate-b-vinyl pyrrolidone) (PHEMA-b-PVP) copolymers with controlled molecular weight and low polydispersity (< 1.4). The thermal behavior and specific interaction of PHEMA-b-PVP diblock copolymers and their corresponding PHEMA/PVP blends were characterized. The result shows that glass transition temperatures of diblock copolymers analysed by differential scanning calorimetry (DSC) are higher than those of the blends. Infrared and solid-state NMR spectroscopic analyses show that hydrogen-bonding interaction of hydroxyl-carbonyl groups of diblock copolymers was also greater than that of the blends. Measurement of the proton spin-lattice relaxation time in the rotating frame, (T-1P(H)), reveals that all diblock copolymers and blends possess one composition-dependent T H, indicating that both diblock copolymers and blends are homogeneous, which is consistent with the DSC analysis. (c) 2006 Elsevier Ltd. All rights reserved.
Polyhedral oligomeric silsesquioxane containing copolymers for negative-type photoresists
(2006-09-22)
Lin, Ho-May
;
Wu, Shi-Yin
;
Huang, Pei-Yuan
;
Huang, Chih-Feng
;
Kuo, Shiao-Wei
A series of methacrylate copolymers containing polyhedral oligomeric silsesquioxane (POSS) was synthesized from the free radical copolymerization of methacrylic acid, methyl methacrylate, and isobutyl propylmethacryl polyhedral oligosilsesquioxanes, and then were modified with glycidyl methacrylate to serve as negative-type photoresists. The UV/Vis spectroscopy reveals that the incorporation of POSS moiety into the copolymer results in a slight decrease in transparency from 99 to 92.5% (at wavelength = 365 nm). The photosensitivity in terms of resist sensitivity (D-n(0.5)), contrast (gamma), and photopolymerization rate are significantly increased with increase in the POSS content. In addition, the induction time is reduced from 0.520 to 0.515 min after incorporating the POSS unit based on photo-DSC analyses. These observed results can be rationalized as due to hydrogen bonding interactions between siloxane and hydroxyl groups in copolymers which tend to attract the methacrylate double bonds surrounding POSS units to crosslink, thereby enhancing the photopolymerization rate and sensitivity. We further evaluate the lithographic property of a photoresist under a collimated exposure.
Syntheses and specific interactions of poly(epsilon-caprolactone)-block-poly(vinyl phenol) copolymers obtained via a combination of ring-opening and atom-transfer radical polymerizations
(2006-11-01)
Kuo, Shiao-Wei
;
Huang, Chih-Feng
;
Lu, Chu-Hua
;
Lin, Ho-May
;
Jeong, Kwang-Un
A series of PCL-b-PVPh diblock copolymers were prepared through combinations of ring-opening and atom-transfer radical polymerizations of c-caprolactone and 4-acetoxystyrene, and subsequent selective hydrolysis of the acetyl protective group. This PCL-b-PVPh diblock copolymer shows a single glass transition temperature over the entire composition range, indicating that this copolymer is able to form a miscible amorphous phase due to the formation of intermolecular hydrogen bonding between the hydroxyl of PVPh and the carbonyl of PCL. In addition, DSC analyses also indicated that the PCL-b-PVPh diblock copolymers have higher glass transition temperatures than their corresponding PCL/PVPh blends. FT-IR was used to study the hydrogen-bonding interaction between the PVPh hydroxyl group and the PCL carbonyl group at various compositions.
Supramolecular micellization of diblock copolymer mixtures mediated by hydrogen bonding for the observation of separated coil and chain aggregation in common solvents
(2008-02-01)
Kuo, Shiao-Wei
;
Tung, Pao-Hsaing
;
Lai, Chih-Ling
;
Jeong, Kwang-Un
;
Chang, Feng-Chih
This paper describes a new approach towards preparing self-assembled hydrogen-bonded complexes that have vesicle and patched spherical structures from two species of block copolymer in non-selective solvents. The assembly of vesicles from the intermolecular complex formed after mixing polystyrene-block-poly(4-vinyl phenol) (PS-b-PVPh) with poly(methyl methacrylate)-block-poly(4-vinylpyridine) (PMMA-b-P4VP) in tetrahydrofuran (THF) is driven by strong hydrogen bonding between the complementary binding sites on the PVPh and P4VP blocks. In contrast, well-defined patched spherical micelles form after blending PS-b-PVPh with weaker hydrogen bonds form between the PVPh and P4VP blocks in DMF, relative to those in THF, which results in the formation of spherical micelles that have compartmentalized coronas that consist of PS and PMMA blocks.
Synthesis and self-assembly of helical polypeptide-random coil amphiphilic diblock copolymer
(2008-05-01)
Kuo, Shiao-Wei
;
Lee, Hsin-Fang
;
Huang, Chih-Feng
;
Huang, Cheng-Jynn
;
Chang, Feng-Chih
Three amphiphilic rod-coil diblock copolymers, poly(2-ethyl-2-oxazoline-b-/-benzyl-L-glutamate) (PEOz-b-PBLG),G), incorporating the same-length PEOz block length and various lengths of their PBLG blocks, were synthesized through a combining of living cationic and N-carboxyanhydride (NCA) ring-opening polymerizations. In the bulk, these block copolymers display thermotropic liquid crystalline behavior. The self-assembled aggregates that formed from these diblock copolymers in aqueous solution exhibited morphologies that differed from those obtained in alpha-helicogenic solvents, that is, solvents in which the PBLG blocks adopt rigid alpha-helix conformations. In aqueous solution, the block copolymers self-assembled into spherical micelles and vesicular aggregates because of their amphiphilic structures. In helicogenic solvents (in this case, toluene and benzyl alcohol), the PEOz-b-PBLG copolymers exhibited rod-coil chain properties, which result in a diverse array of aggregate morphologies (spheres, vesicles, ribbons, and tube nanostructures) and thermoreversible gelation behavior. (C) 2008 Wiley Periodicals, Inc.
Characterization of negative-type photoresists containing polyhedral oligomeric silsesquioxane methacrylate
(2008-07-01)
Lin, Ho-May
;
Hseih, Kuo-Hung
;
Chang, Feng-Chih
;
應用化學系
;
Department of Applied Chemistry
A series of negative-type photoresists made by blending with various contents of polyhedral oligomeric silsesquioxane (POSS) methacrylate were prepared and characterized. These POSS macromers tend to crystallize or aggregate to form their own domains within the photoresist matrix. Sensitivity of the POSS modified photoresist is significantly improved with the increase of the POSS content. Results from photo-DSC analyses indicate that both induction time and peak maximum of heat flux are reduced by blending with POSS macromer. Addition of the proper amount (<13 wt%) of POSS can effectively increase photo-polymerization rate and exothermic heat. Hydrogen bonding interaction between the hydroxyl of photoresist and the siloxane of POSS tends to attract methacrylate double bonds surrounding POSS particles locally and thus enhances the rate of photo-polymerization and sensitivity. (C) 2008 Elsevier B.V. All rights reserved.
Effect of LiClO4 on the thermal and morphological properties of organic/inorganic polymer hybrids
(2008-08-11)
Yen, Ying-Chieh
;
Ye, Yun-Sheng
;
Cheng, Chih-Chia
;
Chen, Hsiu-Mei
;
Sheu, Hwo-Shuenn
This paper describes the thermal properties, morphologies, and interactions within the binary and ternary blends of poly(methyl methacrylate) (PMMA), octa(phenol)octasilsesquioxane (OP-POSS), and LiClO4. In the binary PMMA/OP-POSS blends, the OP-POSS molecules tend to aggregate and result in a decrease (19 degrees C) in the glass transition temperature. In the ternary PMMA/LiClO4/OP-POSS blends, however, the OP-POSS molecules form small sphere-like domains (20 nm) leading to the composite's glass transition temperature increasing by up to 30 degrees C. Based on these FF-IR spectra, the addition of LiClO4 influenced the probability of hydrogen bonds formed between PMMA and OP-POSS and these SEM micrographs, DSC, and XRD data indicated that the addition of LiClO4 is a convenient and simple approach toward dispersing the OP-POSS nanoparticles within PMMA, where the presence of LiClO4 changes the physical effect of OP-POSS from that of a diluent role to a cross-linker role. (c) 2008 Elsevier Ltd. All rights reserved.
The Self-Assembled Structure of the Diblock Copolymer PCL-b-P4VP Transforms Upon Competitive Interactions with Octaphenol Polyhedral Oligomeric Silsesquioxane
(2009-12-16)
Lu, Chu-Hua
;
Kuo, Shiao-Wei
;
Chang, Wen-Teng
;
Chang, Feng-Chih
;
應用化學系
This paper describes the miscibility and self-assembly, mediated by hydrogen-bonding interactions, of new block copolymer/nanoparticle blends. The morphologies adopted by the immiscible poly[(epsilon-caprolactone)-block-(4-vinyl pyridine)] (PCL-b-P4VP) diblock copolymer changes upon increasing the number of competitive hydrogen-bonding interactions after adding increasing amounts of octaphenol polyhedral oligomeric silsesquioxane (OP-POSS). Transmission electron microscopy reveals morphologies that exhibit high degrees of long-range order, such as cylindrical and spherical structures, at relatively low OP-POSS contents, and short-range order or disordered structures at higher OP-POSS contents. Analyses performed using differential scanning calorimetry, wide-angle X-ray diffraction, and FT-IR spectroscopy provide positive evidence that the pyridyl units of the P4VP block are significantly stronger hydrogen-bond acceptors toward the OH group of OP-POSS than are the C=O groups of the PCL block, thereby resulting in excluded and confined PCL phases.
Star Block Copolymers Through Nitroxide-Mediated Radical Polymerization From Polyhedral Oligomeric Silsesquioxane (POSS) Core
(2010-06-15)
Lu, Chu-Hua
;
Wang, Jui-Hsu
;
Chang, Feng-Chih
;
Kuo, Shiao-Wei
;
應用化學系
A series of star block copolymers were prepared through nitroxide-mediated radical polymerization (NMRP) from polyhedral oligomeric silsesquioxanes (POSS) nanoparticle by core-first polymerization. Eight N-alkoxyamine groups were incorporated onto the eight corners of a POSS cube through quantitative hydrosilylation through addition of octakis(dimethylsiloxy)silsesquioxane (O(8)M(8)(H) POSS) with 1-(2-(allyloxy)-1-phenylethoxy)-2,2,6,6-tetramethyl-piperidine (allyl-TEMPO) and Karstedt's agent (a platinum divinylsiloxane complex) was used as a catalyst. Octa-N-alkoxyamines POSS (OT-POSS) were used as platform to synthesize star polystyrene-POSS ((PS)(8)-POSS) homopolymer and diblock copolymers of poly(styrene-block-4-vinyl-pyridine)-POSS ((PS-b-P4VP)(8)-POSS) and poly(styrene-block-acetoxystyrene) ((PS-b-PAS)(8)-POSS) through NMRP. In addition, subsequent selective hydrolysis of the acetyl protective group of (PS-b-PAS)(8)-POSS, the poly(styrene-block-vinyl phenol) ((PS-b-PVPh)(8)-POSS) with strong hydrogen bonding group was obtained. The detailed chemical structure and self-assembled structures of these star block copolymers based on POSS were characterized by (1)H NMR, FTIR, SEC, TEM, and SAXS analyses.

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