• Journal of the Korean Ceramic Society
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• v.29 no.6
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• pp.496-504
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• 1992

Alumina tubes suitable for the support of gas separation membranes have been prepared by the slipcasting technique. These supports have the average pore size of 0.1 ${\mu}{\textrm}{m}$ within the narrow distribution. The sol-gel dipcoating process of nanoparticulate sols is very sensitive to microstructure of the support, and the coating on the inside surface of the tube is found to be more successful than on the outside surface. Nanoparticulate silica sols (0.82 mol/ι) have been synthesized by an interfacial hydrolysis reaction between TEOS and high alkaline water. When coating an alumina tube with these sols, the minimum limits of the particle size and the aging time required for forming the coated gel layer at the given pH are provided. It is optimum to coat the support with less concentrated sols stabilized through aging for the appropriate time (more than 22 days) at the lower pH (pH 2.0) for producing a reproducible crack free thin film coating in composite membranes.

• Journal of the Korean Ceramic Society
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• v.29 no.12
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• pp.970-980
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• 1992

${\gamma}-alumina$ membranes were prepared by sol-gel dip coating or pressurized coating of boehmite sols on slipcasted ${\gamma}-alumina$ support tubes. The particle size of sols synthesized via the modified Yoldas-method could be controlled below 5 mn according to the mole ratio of nitric acid/aluminumtri-sec-butoxide (0.07~1.0). The reproducible crack-free composite membranes were produced by the 2nd dip coating or the pressurized coating technique using very stable sols with the particle size of 45 nm. Nitrogen gas permeability through the top-layer in the composite membrane was about $70~55{\times}10^{-7}\;mol/m^2{\cdot}s{\cdot}Pa$. The thermal stability of the top layer was proved to be good enough upto the heat-treatment temperature of $500^{\circ}C$.

• Korean Chemical Engineering Research
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• v.54 no.6
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• pp.767-774
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• 2016

Three different alumina sols were prepared by hydrolyzing aluminum isopropoxide as a starting material in methanol solvent, followed by peptizing with acetic acid, nitric acid or hydrochloric acid as a peptizing agent by the Sol-Gel Method. Also, coating solutions were obtained by adding a silane coupling agent, (3-glycidyloxypropyl) trimethoxysilane to the alumina sols, deposited on polycarbonate substrates by dip-coating and densified by thermal curing. The effect of types of peptizing agents was studied on the properties of coating films. As a result, coating films, prepared with hydrochloric acid or nitric acid as a peptizing agent, showed excellent properties of pencil hardness of H or 2H and adhesion of 5B. On the other hand, coating films, prepared with acetic acid as a peptizing agent, exhibited poor properties of pencil hardness of HB and adhesion of 3B.

• Korean Chemical Engineering Research
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• v.49 no.3
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• pp.277-284
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• 2011

In this study, UV-curing type organic - inorganic hybrid hard coating solutions were prepared from alumina sols and acrylate monomers. The mixture of alumina sols, prepared from aluminum isopropoxide, and a silane coupling agent, methacryloxypropyl trimethoxysilane(MPTMS), was used as an inorganic component. Also, the mixture of acrylate monomers, pentaerythritol triacrylate(PETA), 1,6-hexanediol diacrylate(HDDA) and dipentaerythritol hexaacrylate (DPEHA), was used as an organic component. The organic-inorganic hybrid coating solutions were obtained by mixing the inorganic component and organic component, deposited on polycarbonate substrates by spin coating and densified by UV-curing. The effect of the amount of MPTMS in the inorganic component and the irradiation time during UV-curing was studied on the properties of coating films. As a result, when 0.20 mole of MPTMS was used, the pencil hardness of coated films showed an excellent pencil hardness of 3H and also exhibited a good abrasion resistance of 2% in haze.

• Journal of the Korean Ceramic Society
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• v.31 no.11
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• pp.1271-1282
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• 1994

The surface of commercial alumina fibers used for reinforcing the MCFC matrix has been coated with ${\gamma}$-LiAlO2 being the same material as the matrix, by the sol-gel method in order to enhance the corrosion resistivity of alumina fibers. Stable LiAlO2 complex polymeric sols for coating was synthesized by mixing aluminum alkoxide polymeric sols with LiNO3 solution. It was found that the LiAlO2 polymeric sol prepared by adding the mixed chelate of acethylacetone and triethanolamine (the mole ratio of AA/TEA = 0.125/0.75) to the 1 mole of the aluminum alkoxide had the excellent stability and coating behavior. The crystalline structure of the dried gel from the ${\gamma}$-LiAlO2 sol was completely transformed into the ${\gamma}$-LiAlO2 at $600^{\circ}C$. The optimum viscosity of the sol for coating the alumina long fibers was 30~40 cP, while it was 12~20 cP in case of the short fiber coating. The ${\gamma}$-LiAlO2 coated alumina fibers without defects fully densified when heat-treated at 120$0^{\circ}C$.

• Proceedings of the Materials Research Society of Korea Conference
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• 1994.05a
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• pp.158-158
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• 1994

• Journal of the Korean Ceramic Society
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• v.29 no.9
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• pp.739-749
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• 1992

The sols prepared by dialyzing solutions, in which the hydrolyzed precipitates of TEOT or directly Ti(OC3H7)4 were resolved, were the nanoparticulate sol with the average particle size less than 7 nm and the anatase crystal phase. In the pH range of 1.5 to 2.9, the particle size of the nanoparticulate TiO2 sols (0.09 mol/ι) increased gradually upto 15 nm~26nm with the increase of pH in the initial aging state but the sols were transparent all the time, and stable without growin any more after 30 days. When the slipcasted porous alumina tubes were coated by the sol-gel dipping method, the minimum particle size and the aging time for forming the coated gel layer at the given pH were optimized. For obtaining the very thin crack-free and reproducible membrane coating, the use of a nanoparticulate TiO2 sol (0.09 mol/ι) aged for about 30 dyas at pH=2.0 was found to be the best.

• Journal of the Korean Ceramic Society
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• v.32 no.1
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• pp.63-70
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• 1995

A crack-free ceramic composite membrane with micropores has been synthesized by the pressurized sol-gel coating technique using the mixed Al2O3-SiO2 sols. The mixed sols were prepared by mixing nanoparticulate SiO2 and boehmite sols. These sols were more stable at lower pH, but very unstable when their copositions were in the range of 50~75mol% of SiO2 at the same pH. The mixed Al2O3-SiO2 membrane prepared from the mixed sol (0.2mol/$\ell$ of solid content and pH=2) containing 40mol% of SiO2 had the mean pore radius of 0.80nm and the specific surface area of 280$m^2$/g. The nitrogen permeability through the coated Al2O3-SiO2 layer was 42$\times$107mol/$m^2$.s.Pa. It was found that the thermal stability of aluminosilicate membranes, even through similar to that of SiO2 membranes, was much improved in comparison with ${\gamma}$-alumina membranes.

• 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.

• Journal of the Korean Ceramic Society
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• v.28 no.2
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• pp.153-159
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• 1991

Polymeric alumina sol and polymeric silica sol were synthesized from aluminum sec-butoxide and tetraethyl orthosilicate, respectively as starting materials. A clear mullite sol was obtained by mixing these sols. When the mullite sol had a proper viscosity which was dependent on drying time, the fibers were fabricated by spinning. The optimum viscosity for fabrication of mullite fibers was 103-104 cps, and the fibers with various sizeswere made using the sols. The mullite was a major phase of the calcined fibers and the diameters of the fibers were about 50$\mu\textrm{m}$.