• Bulletin of the Korean Chemical Society
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• 제32권7호
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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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• 한국신재생에너지학회 2010년도 춘계학술대회 초록집
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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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• 제12권3호
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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.

• 접착 및 계면
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• 제16권1호
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• pp.6-14
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• 2015

본 연구에서는 양친성 반응성 고분자 전구체를 합성하고 이를 사용하여 화학적, 물리적으로 안정한 코아 가교 양친성 고분자(Core-crosslinked Amphiphilic Polymer; 이하 CCAP) 나노입자를 제조하였으며, CCAP 나노입자를 $TiO_2$ 나노입자 제조의 템플레이트로 응용하였다. 먼저 CCAP 나노입자 수용액과 티타늄 이소프로폭사이드(Titanium isopropoxide)를 혼합하여, 매우 안정한 유/무기 나노하이브리드 솔(Sol)을 제조하였으며, 제조된 솔(Sol)은 회전코팅(Spin coating) 기법을 통해 유/무기 하이브리드 박막으로 제조하고, 소결 공정을 통해서 템플레이트인 CCAP를 제거하여 제조된 $TiO_2$ 나노입자의 미세구조를 주사전자현미경(SEM)을 이용하여서 관찰하였다. 다양한 CCAP 나노입자를 템플레이트로 사용하여 제조된 $TiO_2$ 나노입자의 미세구조를 기존 유기물 템플레이트(계면활성제)를 사용하여 제조된 $TiO_2$ 나노입자의 미세구조와 비교하여, CCAP 나노입자가 $TiO_2$ 나노입자 구조에 미치는 영향을 조사하였다.

• Korean Chemical Engineering Research
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• 제53권1호
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• pp.78-82
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• 2015

유기주형(organic template) 입자를 이용하여 소디움실리케이트(sodium silicate)로부터 중공형 실리카(hollow silica) 입자를 제조하였다. 유기주형 입자로는 스티렌 단량체(styrene monomer)로부터 분산중합(dispersion polymerization)에 의해 제조된 폴리스티렌 라텍스(polystyrene latex, PSL) 입자를 사용하였다. 유기주형 입자 제조 시 중합개시제인 2,2'-azobisisobutyronitrile(AIBN)의 주입량을 조절하여 $1{\sim}3{\mu}m$의 크기를 가진 입자를 제조하였다. 생성된 유기주형 입자 표면에 졸-겔(sol-gel)법에 의해 소디움실리케이트로부터 생성된 실리카($SiO_2$) 나노 입자를 코팅하여 PSL/$SiO_2$ 코어-쉘 형태의 입자를 제조하였다. 유기용매인 테트라하이드로푸란(tetrahydrofuran, THF)을 이용하여 코어-쉘 입자 내부의 유기주형을 제거 하였다. 코어-쉘 입자 제조 시 용매의 종류 및 pH의 변화에 따라 생성되는 중공형 실리카 입자의 형상을 조사하였다. PSL/$SiO_2$ 코어-쉘 입자 제조 시 용매를 에탄올에서 물로 변경했을 때 중공형 실리카 입자가 성공적으로 제조되었으며 낮은 pH 값을 갖는 용매에서 쉘 두께가 균일한 중공형 실리카 입자가 형성되었다. 중공형 실리카 입자의 반사도를 측정한 결과 상용 제품(Insuladd)보다 높은 반사 특성을 보여주었다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2010년도 제39회 하계학술대회 초록집
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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.

• 공업화학
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• 제18권2호
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• pp.142-147
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• 2007

본 연구에서는 주형물질로 $C_{16}TMABr$을 이용하여 염기 조건하에서 메조세공을 갖는 산화주석을 졸-겔법으로 합성하였다. 메조세공 $SnO_2$의 합성 최적조건을 탐사하였으며, 얻어진 시료는 X선회절, 질소흡착 및 투과전자현미경 등으로 분석하여 특성을 조사하였다. 금전극과 백금히터 회로를 알루미나 기재상에 스크린 프린팅 법으로 코팅하고, 합성한 메조세공의 산화주석을 전극상에 접합시켜 하나의 유니트로 구성하였으며, 제작한 센서는 $350^{\circ}C$에서 1~10,000 ppm 농도범위의 메탄과 일산화탄소에 대하여 검지능력을 평가하였다. $SnO_2$ 상에 담지된 팔라듐량의 변화가 이들 측정가스의 검출에 미치는 영향도 검토하였다. 메조세공을 갖는 산화주석은 비다공성의 상용 산화주석에 비하여 동일한 측정 조건하에서 측정가스에 대해 보다 높은 감도를 나타낼 뿐 아니라 안정성이 있으면서도 빠른 응답속도를 보였다.

• 대한화장품학회지
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• 제30권2호
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• pp.189-195
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• 2004

카본 블랙은 매우 낮은 밀도로 화장품에는 사용되지 않고 있지만 독성이 없고 안정한 물리적 특성과 검은색의 특성으로 이용 가치가 있다고 사료되는 바이다. 본 연구에서는 TEOS, a) PEO/ lecithin, b) PEO/polyethylene glycol, c) lecithin/polyethylene을 ethanol/water 수용액상에서 계면활성제를 탄화시켜 sol-gei반응에 의해 meso-porous silica샘플을 얻었고 N2 조건하 50$0^{\circ}C$에서 열처리된 organic-inorganic hybrid silica를 합성하였다. Pore안에 카본 블랙을 함유하는 meso-porous silica는 친수성, 소수성 용매에서 모두 좋은 분산성을 보여준다. 이 샘플은 BET에 의해 specific surface area (750$m^2$/g)과 pore size (4-6 nm)이고, XRD측정으로 pore structure (cylindrical type)를, 샘플의 SEM촬영으로 morphology(0.1-0.5$\mu\textrm{m}$ 입자 크기를 갖는 spherical powder)를 갖는다는 것을 알아냈다. 이렇게 합성한 카본-실리카 블랙 컬러를 마스카라에 적용하면 일반적으로 마스카라에 사용되던 블랙 컬러 사용시 보다 좀더 검은색을 보여주는 것은 물론이고 우수한 분산성도 갖는다. 무엇보다 이 파우더의 밀도 조절이 가능하여 마스카라 뿐 만 아니라 모든 화장품에의 사용이 가능하다.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2011년도 춘계학술발표대회
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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.

• 청정기술
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• 제28권1호
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• pp.18-23
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• 2022

에너지 절약을 위한 연구 중 단열 기술 분야에서는 공기의 낮은 열전도도를 활용한 연구가 이뤄지고 있으며 널리 상용화 되고 있다. 본 연구에서는 입자 내부에 공기층을 갖는 중공형(hollow) 형태의 실리카 나노 입자를 제조하여 공기층 크기가 단열 성능에 미치는 영향에 대해 고찰하였다. Polystyrene 주형법을 이용하여 졸-겔공정을 통해 속이 빈 중공형 실리카 나노 입자(Hollow silica nanoparticles)를 제조하였고, 입자를 5 wt %로 도료에 첨가한 후 열전달 실험을 통해 단열 성능을 확인하였다. 기존 페인트에 입자를 혼합하여 약 15 %이상의 단열효율을 나타냈으며, 내부 공기층의 크기가 큰 입자가 작은 입자에 비해 5% 높은 단열 성능을 나타냈다. 이번 연구를 통해 내부 크기에 따른 단열효과의 차이를 보여줌으로써, 중공형 형태의 입자를 첨가제나 도료 제조에 사용하는 경우 단열효과를 높이기 위해 매질 내에서 입자가 공기층을 최대로 이룰 수 있도록 입자의 크기를 고려해야함을 제시한다.