• Bulletin of the Korean Chemical Society
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• v.32 no.7
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• pp.2178-2182
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• 2011

Recently, the synthesis of ordered macroporous materials has received much attention due to its potential use as photonic band gap materials.$^1$ In this study, we have used the three-dimensional (3D) latex array template impregnated with benzenesulfonic acid (BSA), which is capable of catalyzing the reaction using tetraethyl orthosilicate (TEOS) as a precursor and distilled water. The polystyrene (PS) templates were reacted with TEOS in $scCO_2$ at 40 $^{\circ}C$ and at 80 bar. In the reactor, TEOS was filtrated into the PS particle lattice. After the reaction, porous silica materials were obtained by calcinations of the template. The stability test of the PS template in pure $CO_2$ was conducted before the main experiment. Scanning electron microscopy (SEM) images showed that the reaction in $scCO_2$ takes place only on the particle surface. This new method using $scCO_2$ has advantages over conventional sol-gel processes in its capability to control the fluid properties such as viscosity and interfacial tension. It has been found that the reaction in $scCO_2$ occurs only on the particle surface, making the proposed technique as more rapid and sustainable method of synthesizing inverse opal materials than conventional coating processes in the liquid phase and in the vapor phase.

• 한국신재생에너지학회:학술대회논문집
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• 2010.06a
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• pp.64.1-64.1
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• 2010

The morphology of mesoporous $TiO_2$ films plays an important role in the operation of a DSSC. For example, the energy conversion efficiency of DSSCs with well-organized mesoporous $TiO_2$ films is much higher than those with traditional films possessing a random morphology. In previous research, well-organized mesoporous $TiO_2$ films have mainly been synthesized using an amphiphilic block copolymer, e.g., a poly(ethylene oxide) (PEO)-based template. A graft copolymer is more attractive than a block copolymer due to its low cost and the ease with which it can be synthesized. In this work, we provide the first report on the successful synthesis of well-organized mesoporous $TiO_2$ films templated by an organized graft copolymer as a structure directing agent. Well-organized mesoporous $TiO_2$ films with excellent channel connectivities were developed via the sol gel processusing an organized PVC-g-POEM graft copolymer synthesized by one-pot ATRP. The careful adjustment of copolymer composition and solvent affinity using a THF/$H_2O$/HCl mixture was used to systematically vary the material structure. The influence of the material structure on solar cell performance was then investigated. A solid-state DSSC employing both the graft copolymer templated organized 700 nm-thick $TiO_2$ films and graft copolymer electrolytes exhibited a solar conversion efficiency of 2.2% at 100 $mW/cm^2$. This value was approximately two-fold higher than that attained from a DSSC employing a random mesoporous $TiO_2$ film. The solar cell performance was maximized at 4.6% when the film thickness was increased to $2.5{\mu}m$. We believe that this graft copolymer-directed approach introduces a new and simple route toward the synthesis of well-organized metal oxide films as an alternative to a conventional block copolymer-based template.

• Transactions on Electrical and Electronic Materials
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• v.12 no.3
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• pp.119-122
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• 2011

A series of mesoporous silicalites was synthesized using different compositions of tetraethylorthosilicate and methyltriethoxysilane (MTES) as the silica source. Cetyltrimethylammonium bromide was used as the organic template. Their detailed pore structures were investigated by transmission electron microscopy, X-ray diffraction, and N2 adsorption method. The thermal properties of these silicalites were studied by thermogravimetric analysis. The increased amount of MTES destroyed mesoporous channels and reduced pore sizes from 3.4 nm to 2.8 nm in calcined silicalites. The calcined silicalite transformed completely into an amorphous state at 30% MTES loading. Methyl pending groups of MTES hindered the structural ordering of ≡Si-O- frameworks, resulting in an amorphous structure. This was caused by the insufficient formation of supramolecular assembly with the organic template. No capillary condensation step was found in MS 7/3 silicalite. The other capillary condensation steps shifted toward the lower relative pressure with increasing MTES content, indicating the reduction of pore sizes.

• Journal of Adhesion and Interface
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• v.16 no.1
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• pp.6-14
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• 2015

In this study, physically and chemically stable core-crosslinked amphiphilic polymer (CCAP) nanoparticles were prepared using amphiphilic reactive precursors via soap-free emulsion process. Obtained CCAP nanoparticles were used as templates for synthesis of nanostructured $TiO_2$ nanoparticles. First, CCAP nanoparticles dispersed aqueous solutions were mixed with titanium isopropoxide to prepare stable organic-inorganic hybrid sols, and then obtained sols were spin coated onto glass substrate to prepare hybrid thin films onto glass, and then hybrid thin films were calcinated at various temperature to remove CCAP. Nanostructure of calcinated thin fims were examined by SEM. To study effect of CCAP nanoparticles on nanostructure of $TiO_2$ nanoparticles, the morphology of $TiO_2$ nanoparticles prepared using various CCAP templates was compared with that of $TiO_2$ nanoparticles prepared using conventional organic template, nonionic surfactant, Triton X-100.

• Korean Chemical Engineering Research
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• v.53 no.1
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• pp.78-82
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• 2015

Hollow silica particles were prepared using sodium silicate and organic templates. Polystyrene latex (PSL) particles produced by dispersion polymerization were used as organic templates. PSL particles ranged from $1{\mu}m$ to $3{\mu}m$ in diameter were synthesized by adjusting the amount of 2,2'-azobisisobutyronitrile (AIBN). The PSL/$SiO_2$ core-shell particles were prepared by coating of silica nanoparticles originated from sodium silicate using sol-gel method. The organic templates were removed by the organic solvent, tetrahydrofuran (THF). Morphology of hollow silica particles was investigated with respect to types of the reaction medium and pH during the process. By changing the solvent from ethanol to water, hollow silica particles were successfully formed. Hollow silica particles with the uniform shell thickness were produced at low pH as well. The reflectivity of the as-prepared silica particles was measured in the range of the wavelength of UV and visible light. Hollow silica particles showed much better reflective properties than the commercial light reflector, Insuladd.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.08a
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• pp.281-281
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• 2010

Very low refractive index (<1.4) materials have been proved to be the key factor improving the performance of various optical components, such as reflectors, filters, photonic crystals, LEDs, and solar cell. Highly porous SiO2 are logically designed for ultralow refractive index materials because of the direct relation between porosity and index of refraction. Among them, ordered macroporous SiO2 is of potential material since their theoretically low refractive index ~1.10. However, in the conventional synthesis of ordered macroporous SiO2, the time required for the crystallization of organic nanoparticles, such as polystyrene (PS), from colloidal solution into well ordered template is typical long (several days for 1 cm substrate) due to the low interaction between particles and particle - substrate. In this study, polystyrene - polyacrylic acid (PS-AA) nanoparticles synthesized by miniemulsion polymerization method have hydrophilic polyacrylic acid tails on the surface of particles which increase the interaction between particle and with substrate giving rise to the formation of PS-AA film by simply spin - coating method. Less ordered with controlled thickness films of PS-AA on silicon wafer were successfully fabricated by changing the spinning speed or concentration of colloidal solution, as confirmed by FE-SEM. Based on these template films, a series of macroporous SiO2 films whose thicknesses varied from 300nm to ~1000nm were fabricated either by conventional sol - gel infiltration or gas phase deposition followed by thermal removal of organic template. Formations of SiO2 films consist of interconnected air balls with size ~100 nm were confirmed by FE-SEM and TEM. These highly porous SiO2 show very low refractive indices (<1.18) over a wide range of wavelength (from 200 to 1000nm) as shown by SE measurement. Refraction indices of SiO2 films at 633nm reported here are of ~1.10 which, to our best knowledge, are among the lowest values having been announced.

• Applied Chemistry for Engineering
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• v.18 no.2
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• pp.142-147
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• 2007

In this study, mesoporous tin oxide was synthesized by sol-gel method using $C_{16}TMABr$ surfactant as a template in a basic condition. The optimum conditions for the synthesis of mesoporous $SnO_2$ were investigated and the obtained samples were characterized by XRD, nitrogen adsorption and TEM analysis. A mesoporous and nanostructured $SnO_2$ gas sensor with Au electrode and Pt heater has been fabricated on alumina substrate as one unit via a screen printing process. Sensing abilities of fabricated sensors were examined for CO and $CH_4$ gases, respectively, at $350^{\circ}C$ in the concentration range of 1~10,000 ppm. Influence of loading amount of palladium impregnated on $SnO_2$ was also tested in detection of those gases. High sensitivity to detecting gases and the fast response speed with stability were obtained with the mesoporous tin oxide sensor as compared to a non-porous one under the same detection conditions.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.30 no.2
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• pp.189-195
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• 2004

Carbon black have not been used as pigment material in cosmetic because of very low density and dispersity, but carbon black have applicable character as black pigment because of non-toxic, stable physico-chemical property, and black colority. In this study, mesoporous silica samples were synthesized by sol-gel reaction using surfactants-template method; TEOS (tetraethoxysilane) - a) PEO/lecithin, b) PEO/polyethylene glycol, c) lecithin/polyethylene glycol in ethanol/water solution. Synthesized organic-inorganic hybrid - silica were heat-treated in N2 condition at 500$^{\circ}C$. Mesoporous silica with black carbon in pore have the effective density and show the good dispersity in both hydrophilic and hydrophobic solvent. Properties of the samples were measured; specific surface area (750㎡/g) and pore size (4-6nm) using BET, pore structure (cylindrical type) using XRD, morphology (spherical powder with 0.1-0.5$\mu\textrm{m}$ partical size) of the samples using SEM. Carbon-silica black color applied to mascara, it shows a dark black colority and good dispersity as compared with the general black color titania pigment. Moreover, it is possible to control the density of black color pigment because it is possible to control pore volume and particle size of mesoporous silica properly. It show the good volume effects in mascara. That is why possible to apply all kinds of cosmetic products.

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.05a
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• pp.8.1-8.1
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• 2011

Nanocrystalline titanium dioxide ($TiO_2$) materials have been widely used as an electron collector in DSSC. This is required to have an extremely high porosity and surface area such that the dye can be sufficiently adsorbed and be electronically interconnected, resulting in the generation of a high photocurrent within cells. In particular, their geometrical structures and crystalline phase have been extensively investigated as important issues in improving its photovoltaic efficiency. In this study, we present a new strategy to fabricate a photoelectrode having a periodic structured $TiO_2$ film templated from 1D or 3D polystyrene (PS) microspheres array. Monodisperse PS spheres of various radiuses were used for colloidal array on FTO glasses and two types of photoelectrode structures with different $TiO_2$ materials were investigated respectively. One is the igloo-shaped electrode prepared by $TiO_2$ deposition by RF-sputtering onto 2D microsphere-templated substrates. At the interface between the film and substrate, there are voids formed by the decomposition of PS microspheres during the calcination step. These holes might be expected to play the predominant roles as scattering spherical voids to promote a light harvesting effect, a spacious structure for electrolytes with higher viscosity and effective paths for electron transfer. Additionally the nanocrystalline $TiO_2$ phase prepared by the RF-sputtering method was previously reported to improve the electron drift mobility within $TiO_2$ electrodes. This yields solar cells with a cell efficiency of 2.45% or more at AM 1.5 illumination, which is a very remarkable result, considering its $TiO_2$ electrode thickness (<2 ${\mu}m$). This study can be expanded to obtain higher cell efficiency by higher dye loading through the increase of surface area or multi-layered stacking. The other is the inverse opal photonic crystal electrode prepared by titania particles infusion within 3D colloidal arrays. To obtain the enlargement of ordered area and high quality of crystallinity, the synthesis of titania particles coated with a organic thin layer were applied instead of sol-gel process using the $TiO_2$ precursors. They were dispersed so well in most solvents without aggregates and infused successfully within colloidal array structures. This ordered mesoporous structure provides the large surface area leading to the enough adsorption of dye molecules and have an light harvesting effect due to the photonic band gap properties (back-and-forth reflection effects within structures). A major advantage of this colloidal array template method is that the pore size and its distribution within $TiO_2$ photoelectrodes are determined by those of latex beads, which can be controlled easily. These materials may have promising potentials for future applications of membrane, sensor and so on as well as solar cells.

• Clean Technology
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• v.28 no.1
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• pp.18-23
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• 2022

Using air as an insulator due to its low heat transfer coefficient has been studied and has been widely commercialized to save energy in the field of thermal insulation technology. In this study, we analyzed the heat insulating effect of hollow silica nanoparticles mixed in non-uniform size, and the maximum heat insulating efficiency of these particles given the limited number of particles that can be mixed with a medium such as paint. The hollow silica nanoparticles were synthesized via a sol-gel process using a polystyrene template in order to produce an air layer inside of the particles. After synthesis, the particles were analyzed for their insulation effect according to the size of the air layer by adding 5 wt % of the particles to paint and investigating the thermal insulation performance by a heat transfer experiment. When mixing the particles with white paint, the insulation efficiency was 15% or higher. Furthermore, the large particles, which had a large internal air layer, showed a 5% higher insulation performance than the small particles. By observing the difference in the insulation effect according to the internal air layer size of hollow silica nanoparticles, this research suggests that when using hollow particles as a paint additive, the particle size needs to be considered in order to maximize the air layer in the paint.