• Bulletin of the Korean Chemical Society
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• v.34 no.9
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• pp.2747-2752
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• 2013

Surface modification of colloidal silica nanoparticles without disrupting the electric double layer of nanoparticles is a major challenge. In the work, silane was employed to modify colloidal silica nanoparticles without inducing bridge flocculation obviously. The effect of pH value of the silica sol, the amount of silane in feed, and reaction temperature on the graft amount and the final size of modified particles was investigated. The increased weight loss by TG and the appearance of $T_2$ and $T_3$ except for $Q_2$ and $Q_3$ signals by CP/MAS $^{29}Si$ NMR of the modified samples verified the successful grafting of silane. The graft amount reached 0.57 mmol/g, which was slightly lower than theory value, and the particle size remained nearly the same as unmodified particles for acidic silica sol at the optimum condition. For alkaline silica sol after modification, aggregates composed of several nanoparticles connected together with silane moleculars as the bridge appeared.

• Proceedings of the Materials Research Society of Korea Conference
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• 2010.05a
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• pp.6.2-6.2
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• 2010

Stainless steel is widely known to have superior corrosion properties. However, in some harsh conditions it still suffers various kinds of corrosions such as galvanic corrosion, pitting corrosion, intergranular corrosion, chloride stress corrosion cracking, and etc. For the corrosion protection of stainless steel, the ceramic coatings such as protective silica film can be used. The sol-gel coating technique for the silica film has been extensively studied especially because of the cost effectiveness. It has been proved that silica can improve the oxidation and the acidic corrosion resistance of metal surface in a wide range of temperatures due to its high heat and chemical resistance. However, in the sol-gel coating process there used to engage a heat treatment at an elevated temperature like $500^{\circ}C{\sim}600^{\circ}C$ where cracks in the silica film would be formed because of the thermal expansion mismatch with the metal. The cracks and pores of the film would deteriorate the corrosion resistance. When the heat treatment temperature is reduced while keeping the adhesion and the density of the film, it could possibly give the enhanced corrosion resistance. In this respect, inorganic protective silica film was tried on the surface of stainless steel using a sol-gel chemical route where silica nanoparticles, tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES) were used. Silica nanoparticles with different sizes were mixed and then the film was deposited on the stainless steel substrate. It was intended by mixing the small and the large particles at the same time a sufficient consolidation of the film is possible because of the high surface activity of the small nanoparticles and a modest silica film is obtained with a low temperature heat treatment at as low as $200^{\circ}C$. The prepared film showed enhanced adhesion when compared with a silica film without nanoparticle addition. The films also showed improved protect ability against corrosion.

• Textile Coloration and Finishing
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• v.21 no.6
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• pp.1-11
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• 2009

Super-hydrophobic surface, with a water contact angle greater than $150^{\circ}$, has a self cleaning effect termed 'lotus effect'. We introduced super-hydrophobicity onto aramid/rayon mixture fabric with dual-scale structure by assembling silica nano-sol. Mixture fabric was treated with silica nano-sol, fluoric polymer using various parameters such as particle size, concentration. Silica nano-sol size were measured using particle size analyzer. Morphological changes by particle size were observed using field emission scanning electron microscopy(FE-SEM), contact angle measurement equipment. The contact angle of water was about $134.0^{\circ}$, $137.0^{\circ}$, $143.0^{\circ}$, $139.5^{\circ}$ and $139.0^{\circ}$ for mixture fabric coated with 100.2nm, 313.7nm, 558.2nm, 628.5nm and 965.4nm silica nano-sol, compared with about $120.0^{\circ}$ for mixture fabric coated with fluoric polymer. When we mixed particle sizes of 100.2nm and 558.2nm by 7:3 volume ratio, the contact angle of water was about $146.2^{\circ}$. And we mixed particle sizes of 313.7nm and 558.2nm by 7:3 volume ratio, the contact angle of water was about $141.8^{\circ}$. Also we mixed particle sizes of 558.2nm and 965.4nm by 7:3 volume ratio, the best super-hydrophobicity was obtained. In this paper, we fabricated the water-repellent surfaces with various surface structures by using four types of silica nano-sol, and we found that the dual-scale structure was very important for the super-hydrophobicity.

• Journal of the Korean Ceramic Society
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• v.28 no.6
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• pp.488-494
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• 1991

In this study, the effects of catalyst and DCCA content were investigated in order to determine the optimum conditions of monolithic silica gel formation through sol-gel process. Formamide, oxalic acid, glycerol and dimethylformamide are used as DCCA. To observe the phenomena in drying and heat-treating of gels, we examined structural exchange of gels using FT-IR, TG-DTA and XRD. Monolithic gels were obtained by adding formamide and dimethylformamide as DCCA. According to the heat treatment schedule, silica glass is prepared by heat-treatment up to 1050$^{\circ}C$.

• Journal of the Korean Ceramic Society
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• v.34 no.9
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• pp.993-1001
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• 1997

The (0.8PPV+0.2DMPPV) copolymer and silica/borosilicate composites were synthesized by sol-gel process. The organic-inorganic hybrid solution was prepared by using of (0.8PPV+0.2DMPPV) copolymer precursor solution as a raw material for organic components and TEOS and TMB for glass components. Then by drying the solution in vacuum at 5$0^{\circ}C$ for 7days and subsequent heat treatment in vacuum at 15$0^{\circ}C$~30$0^{\circ}C$ for 2h~72h with heating rate of 0.2$^{\circ}C$/min and 1.8$^{\circ}C$/min, the organic-inorganic composites were synthesized. Microstructural evolution of the composites was characterized by DSC, IR spectrocopy, UV/VIS spectroscopy, and TEM. Elimination of the polymer precursor and degradation of the polymer were observed by DSC and Si-O and trans C=C absorption peaks were identified by IR spectra. The polymer was found to be successfully incorporated into the glass matrix and it was confirmed by the absorption peaks from the polymer in the UV/VIS spectra and the TEM results. The absorption peak of the composites was found to shift toward short wavelength side compared to that of the pure polymer and the amount of the blue shift increased with increasing the heat treatment temperature and heat treatment time and with decreasing the heating rate.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.96-96
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• 2010

Monodispersed spherical silica-coated ceria nanoparticles were prepared through a sol-gel process using tetraethylorthosilicate (TEOS) and ceria fine particles. In this process, ceria fine particles were also prepared from cerium nitrate. The mean size of ceria particles was 300nm. Silica nanoparticles with narrow particle size distribution were prepared by controlled hydrolysis of TEOS solution. The silica sols were obtained by peptization, the process of redispersing a coagulated colloid, and were coated on ceria particles by the control of the weight ratio of silica/ceria and the pH of the mixture in aqueous solution. The morphologies of particles were characterized with scaning electron microscopy(SEM), transmission electron microscopy(TEM) and atomic force microscopy(AFM). The coating thickness of silica particles obtained by using this method was controlled in the range of 30 - 70nm.

• Korean Chemical Engineering Research
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• v.45 no.5
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• pp.442-447
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• 2007

In order to improve the surface hardness of transparent plastic films, organic-inorganic hybrid coating solutions were synthesized by the sol-gel method. The coating solutions were prepared by adding GPTMS (glycidoxypropyl trimethoxysilane) to a colloidal silica (12 nm) suspension. PC(polycarbonate) substrates were dipped into the coating solutions and dried at room temperature for 10 min before being cured at $80^{\circ}C$ for 30 min. The effect of the solution pH and GPTMS content was investigated on the properties of coating films. The pencil hardness and adhesion to substrates of the coating films, prepared at acidic condition (pH 4), showed better properties than those at neutral or basic conditions. Also, the pencil hardness and adhesion to substrates of the coating films increased with increasing GPTMS content.

• Journal of the Korean Ceramic Society
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• v.36 no.9
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• pp.893-900
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• 1999

Silica films were prepared on Si single crystal substrates by sol-gel process using TEOS as starting materials. Films were fabricated by a spin coating technique. Sol solutions were prepared by varying the compositions of CH3OH, H2O and DMF with fixed molar ratio of TEOS=1, HCl=0.05(mol). Wetting behavior viscosity of solutions gelation time thickness of films and cracking behavior were investigated with the various solution compositions. Wetting behaviors of solutions depended on the solution compositions mixing method and mixing rate. The optimum composition of sol was TEOS : DMF ; CH3OH: H2O :HCl=1:2:4:4:0.05(mol) and the mixing rate of solution was optimized at 1 ml/min. Viscosity of solutions were controlled by choosing a reaction time(elapsed time after mixing) at a room temperature so that we could get up to 800nm thick film The surface roughness was getting poor when thickness of films was thicker than 500nm. Thickness of coated films were increased with decreasing amount of CH3OH. The best surface roughness was obtained at the content of CH3OH 4 mol. The shortest gelation time was obtained with the content of CH3OH 8 mol. Crack-free filkms were fabricated when sintered at 500$^{\circ}C$ for 1 hr with heating rate of 0.6$^{\circ}C$/min.

• Proceedings of the Polymer Society of Korea Conference
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• 2006.10a
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• pp.233-233
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• 2006

[ $Y_{2}O_{2}S:Eu$ ], a red phosphor, coated with silica nanoparticles or nanocomposites composed of silica nanoparticles and polymeric materials such as PMMA and PVP was prepared via sol-gel process. Samples were prepared from four different methods coded P1, P2, P3, and P4. P1 includes a conventional sol-gel process and a dip-coating method while P2 has the same procedure with P1 except that nanocomposites containing both silica nanoparticles and polymer prepared by sol-gel process were used as coating materials. In P3 method, phosphors were dispersed in a solution containing silica precursor, i.e., TEOS and then polymerization was performed to coat onto the phosphors surface while P4 followed the same procedure with P3 except that a solution containing both TEOS and organic monomer were used in preparing coating materials. Among various coating methods examined in this study, uniform coating of phosphor could be achieved by using method P4, i.e., phosphor surface coating in a solution containing hydrophobic monomer and TEOS. Furthermore, $Y_{2}O_{2}S:Eu$ red phosphor coated with nanocomposite composed of PMMA matrix and silica nanoparticles exhibited enhanced PL intensity and long-term stability.

• Korean Chemical Engineering Research
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• v.48 no.4
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• pp.428-433
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• 2010

Waterborne polyurethane(WPU) was synthesized from isophorone diisocyanate(IPDI), poly(tetramethylene glycol)(PTMG), dimethylol propionic acid(DMPA), triethylamine(TEA), ethylenediamine(EDA) and 3-aminopropyl triethoxysilane(APS) as a coupling agent. Subsequently, WPU/silica nanocomposites with different silica contents(0 to 8 wt%) were prepared by performing sol-gel reactions with tetraethylorthosilicate in the WPU matrix. The average particle size of the nanocomposite solutions increased with increasing TEOS content. Also, the prepared nanocomposites showed better thermal stability than pure WPU.