• Title/Summary/Keyword: Sol-gel polycondensation

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Synthesis of Organic-Inorganic Nanohybrids Using Epoxy-Functionalized Alkoxysilane and Their Properties (Epoxy-Functionalized Alkoxysilane을 이용한 Organic-Inorganic Nanohybrids합성과 물성)

  • Kim, Bo-Young;Kim, Juyoung
    • Journal of Adhesion and Interface
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    • v.15 no.2
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    • pp.69-76
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    • 2014
  • Two kinds of epoxy-functionalized alkoxysilane (EAS) compounds (EAS-MS and EAS-ES) were successfully synthesized through the reaction between epoxy resin (YD-128) and aminopropyl trimethoxysilane (APTMS) or aminopropyl triethoxysilane (APTES). By the hydrolysis-polycondensation reaction of EAS compounds with 3-Glycidyloxypropyl trimethoxysilane (GPTMS) and Tetraethyl orthosilicate (TEOS), silica/epoxy nanohybrids could be prepared at various compositions of EAS to GPTMS/TEOS. Prepared nanohybrids were yellow transparent and miscible with various organic solvents. By the reaction silica/epoxy nanohybrids with curing agents (TETA or acrylic acid), cured hybrids films could be obtained. These cured films showed higher thermal stability and mechanical property compared to cured neat epoxy resin. TEM and AFM images showed formation of nano-sized silica nanoparticles within cured hybrid films.

Organic-inorganic Nano Composite Membranes of Sulfonated Poly(Ether Sulfone-ketone) Copolymer and $SiO_2$ for Fuel Cell Application

  • Lee, Dong-Hoon;Park, Hye-Suk;Seo, Dong-Wan;Kim, Whan-Gi
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2006.09a
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    • pp.487-488
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    • 2006
  • Novel bisphenol-based wholly aromatic poly(ether sulfone-ketone) copolymer containing pendant sulfonate groups were prepared by direct aromatic nucleophilic substitution polycondensation of 4,4-difluorobenzophenone, 2,2'-disodiumsulfonyl-4,4'-fluorophenylsulfone (40mole% of bisphenol A) and bisphenol A. Polymerization proceeded quantitatively to high molecular weight in N-methyl-2-pyrrolidinone at $180^{\circ}C$. Organic-inorganic composite membranes were obtained by mixing organic polymers with hydrophilic $SiO_2$ (ca. 20nm) obtained by sol-gel process. The polymer and a series of composite membranes were studied by FT-IR, $^1HNMR$, differential scanning calorimetry (DSC) and thermal stability. The proton conductivity as a function of temperature decreased as $SiO_2$ content increased, but methanol permeability decreased. The nano composite membranes were found to posse all requisite properties; Ion exchange capacity (1.2meq./g), glass transition temperatures $(164-183\;^{\circ}C)$, and low affinity towards methanol $(4.63-1.08{\times}10^{-7}\;cm^2/S)$.

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Low Temperature Preparation of Transparent Glass-Ceramic Using Metal-Alkoxides (1) Synthesis and Properties of Porous Monolithic Gel in Li2O·1.7Al2O3·8.6SiO2 (금속 알콕시드를 이용한 투명 결정화유리의 저온 합성 (1) Li2O·1.7Al2O3·8.6SiO2 다공성 겔체의 합성)

  • Chun, Kyung-Soo;Tak, Joong-Jae
    • Applied Chemistry for Engineering
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    • v.18 no.6
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    • pp.568-574
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    • 2007
  • Crack-free dried gel monoliths of the composition $Li_2O1{\cdot}7Al_2O_3{\cdot}8.6SiO_2$ have been prepared as a precursor of transparent glass-ceramic by the hydrolysis and polycondensation of mixed metal alkoxides in solutions containing N,N-dimethylformamide as the drying control chemical additive, alcohols, and water. It was investigated that activation energy for gelation according to the variation of water concentration ranged from 13 to 14 kcal/mol. Only when the amount of water for gelation was 3 times higher than the stoichiometric amount, monolithic dry gels were successfully prepared after drying at $70{\sim}75^{\circ}C$ and at a rate of 0.1~0.3%/h. The specific surface area, the pore volume, the average pore diameters of dried gel at $180^{\circ}C$ were about $239.40m^2/g$, 0.001~0.03 mL/g, and $145.62{\AA}$, respectively. It showed that the dried monolithic gel had a porous body. The DTA curve had the first exothermic peak around $800^{\circ}C$ and the 2nd peak around $980^{\circ}C$, which may correspond to crystallization of the gel.

A Study on the Preparation of Aluina & Titania Sols for Coatings (코팅용 알루미타, 티타니아솔 제조에 관한 연구)

  • Kim, Chu-Hui;Choe, Hyeong-Su;Jo, Yeong-Sang;Im, Jong-Ju
    • Korean Journal of Materials Research
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    • v.4 no.3
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    • pp.319-328
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    • 1994
  • Aluminium and titanium precursors containing $\beta$-diketonate ligands were used for the synthesis of polymeric sols of alumina and titania by sol-gel methods. To prepare polymeric sols by solgel processing, we synthesized modified precursors having chelating organic ligands. With these precursors it was found to be possible to control both hydrolysis and polycondensation reaction rates which resulted in ultrafine particles few nms of average size. The optimum molar ratio of acid to alkoxide for alumina sol was 0.3-0.4 and that of water to alkoxide &as 1. On the other hand, the corresponding ratios for titania sol were found be 0.25-0.20 and 1 respectively. Dynamic light scattering measurements indicated that the average particle size in both sols was in the order of few nms. SEM photographs were taken to observe crack-free and smooth surfaces of coated membranes after sintering at $450^{\circ}C$. Alumina coated membrane on a slide glass had about 4-4.5$\mu \textrm{m}$, thickness and titania coated one had 2-2.5$\mu \textrm{m}$, thickness. And according to TEM photographs, the grain size of titania was smaller than 30nm and that of alumina was in the range of few $\AA$s to 2nms. An X-ray diffraction study revealed that alumina was $\gamma$ phase and titania was anatase crystal.

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