• 한국세라믹학회지
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• 제41권7호
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• pp.528-533
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• 2004

입자크기가 20∼700nm인 구형 실리카입자의 자연침강 혹은 원심분리법으로 제조한 주형체에 탄화규소 전구체 polymethyl-silane (PMS) 혹은 polycarbosilane (PCS) 고분자 용액을 함침한다음, 가교 및 1000∼140$0^{\circ}C$ 열분해하고 마지막으로 불산 (HF)으로 실리카를 식각하여 84∼658nm 기공이 3차원으로 정렬된 메크로다공성(macroporous) 탄화규소 세라믹과 불규칙적인 15∼65nm 기공을 가진 메조다공성(mesoporous) 탄화규소 세라믹을 제조하였다. 전자는 112nm 실리카 입자 주형체를 사용하여 140$0^{\circ}C$로 처리했을 때, 표면적 584.64$m^2$g$^{-1}$을 나타낸 반면, 후자는 20-30nm 실리카 주형체를 사용하여 100$0^{\circ}C$로 처리하였을때, 최대의 표면적 619.4$m^2$g$^{-1}$를 나타내었다, 이와 같이 사용된 실리카 입자, 고분자 전구체, 그리고 열처리 조건에 따른 기공특성을 SEM. TEM 및 BET으로 분석 설명하였다.

• 한국지반환경공학회 논문집
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• 제13권6호
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• pp.27-31
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• 2012

본 연구에서는 지하수 내의 BTEX 제거를 위한 흡착제로서 다양한 관능기화 메조포러스 실리카를 검토하였다. BTEX 물질로는 파라자일렌이 사용되었다. 관능기화 메조포러스 실리카는 공중합을 통해 MCM-41 기반 구조에 모노아민, 트리아민, 니트릴, 페닐, 옥틸기를 부착하여 합성되었다. 관능기화 메조포러스 실리카에서 파라자일렌 흡착 부위로 작용하는 부위는 Si-O-Si 결합, 계면활성제, 관능기인 것으로 사료된다. 관능기화 메조포러스 실리카의 자일렌 흡착능을 비교한 결과, 옥틸기를 부착한 경우에 MCM-41에 비해 자일렌 흡착능이 향상되었으며, 계면활성제로는 stearyltrimethylammonium chloride(STMACl)가 cetyltrimethylammonium bromide(CTMABr)에 비해 우수하였다. MCM-41을 기본 구조로, 옥틸기를 관능기로, STMACl을 계면활성제로 사용한 메조포러스 실리카는 $20^{\circ}C$에서 Langmuir model 상에서 최대 4.17 mmol/g의 최대 흡착량을 가질 것으로 평가되었으며, 이는 MCM-41에 비해 약 2.9배 높은 수치였다.

• 전기화학회지
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• 제17권2호
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• pp.86-93
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• 2014

5 nm의 중형기공(mesopore)을 지녔으며 5~7 nm 굵기의 산화주석($SnO_2$) 나노선 다발이 잘 정렬된 meso-$SnO_2$를 주형합성법을 이용해서 제조하였다. 또한 주형합성법을 변형시켜서 5~7 nm 굵기의 동일한 나노선 다발 사이에 존재하는 중형기공에 주형으로 사용되었던 실리카($SiO_2$)를 일부 남긴 meso-$SnO_2$와 실리카의 복합체인 meso-$SnO_2$/$SiO_2$도 제조하였다. X-선 회절, 질소흡착법, 투과전자현미경을 이용해서 meso-$SnO_2$와 meso-$SnO_2$/$SiO_2$의 구조를 확인하였다. meso-$SnO_2$/$SiO_2$는 meso-$SnO_2$에 비해서 충방전시 발생하는 부피 팽창을 완화할 수 있을 것으로 예측했으며, 순환전압전류곡선, 교류 임피던스 분석, 충방전 전압 Profile 변화를 통해 부피 팽창 완화 효과를 확인하였다. 하지만, 수명 특성 측면에서는 구조 제어 효과가 미비하여, 향후 이를 개선하는 연구가 진행되어야 한다.

• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3712-3719
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• 2011

Confined Pt and $CoFe_2O_4$ nanoparticles (NPs) in a mesoporous core/shell silica microsphere, Pt-$CoFe_2O_4$@meso-$SiO_2$, were prepared using a bi-functional linker molecule. A large number of Pt NPs in Pt-$CoFe_2O_4$@meso-$SiO_2$, ranging from 5 to 8 nm, are embedded into the shell and some of them are in close contact with $CoFe_2O_4$ NPs. The hydrogenation of cyclohexene over the Pt-$CoFe_2O_4$@meso-$SiO_2$ microsphere at $25^{\circ}C$ and 1 atm of $H_2$ yields cyclohexane as a major product. In addition, it gives oxygenated products. Control experiments with $^{18}O$-labelled water and acetone suggest that surface-bound oxygen atoms in $CoFe_2O_4$ are associated with the formation of the oxygenated products. This oxidation reaction is operative only if $CoFe_2O_4$ and Pt NPs are in close contact. The Pt-$CoFe_2O_4$@meso-$SiO_2$ catalyst is separated simply by a magnet, which can be re-used without affecting the catalytic efficiency.

• Bulletin of the Korean Chemical Society
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• 제26권3호
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• pp.418-422
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• 2005

By introducing spin-coating method to the evaporation induced self-assembly (EISA) process, a simple and reproducible route in controlling the mesophase of silica thin films has been developed for the first time in this work. When a comparatively solvent-rich Si-sol (The atomic ratio of TEOS : F127 : HCl : $H_2O$ : EtOH = 1 : 0.006 : 0.2 : 9.2 : 30) was used as coating solution, the mesophase of resultant silica films was selectively controlled by adjusting the spin-on speed. The cubic mesophase has been obtained from the coating at a low rpm, such as 600 rpm, while the 2-D hexagonal mesophase is formed at a high rpm, such as 2,500 rpm. At a medium coating speed, a mixture of cubic and hexagonal mesophase has been found in the fabricated films. The present results confirm that the evaporation rate of volatile components at initial step is critical for the determination of mesopore structures during the EISA process.

• Bulletin of the Korean Chemical Society
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• 제25권5호
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• pp.634-638
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• 2004

Titanium silicalite-1 (TS-1) molecular sieve was produced by microwave heating of amorphous titanium-containing solid precursors after impregnation with aqueous TPAOH solution. $SiO_2-TiO_2$ xerogel, sub-micron sized $SiO_2-TiO_2$ prepared by thermal plasma process, and Ti-containing mesoporous silica, Ti-HMS, were tested as the solid phase substrates. Highly crystalline product was obtained within 30 min. after microwave irradiation with yields over 90% using $SiO_2-TiO_2$ xerogel, which showed essentially identical physicochemical properties to TS-1 prepared by conventional hydrothermal method. Excellent catalytic activity was also obtained for 1-hexene epoxidation using $H_2O_2.\;SiO_2-TiO_2$ particles prepared by thermal plasma and Ti-HMS were found inferior as a substrate for TS-1, probably due to difficulties in wetting the surface uniformly with TPAOH.

• Korean Membrane Journal
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• 제6권1호
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• pp.16-23
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• 2004

The silica containing carbon (C-SiO$_2$) membranes were fabricated using poly(imide siloxane) (PIS) having -CO- swivel group. The characteristics of porous C-SiO$_2$ structures prepared by the pyrolysis of poly(imide siloxane) were related with the micro-phase separation between the imide block and the siloxane block. Furthermore, the nitrogen adsorption isotherms of the CMS and the C-SiO$_2$ membranes were investigated to define the characteristics of porous structures. The C-SiO$_2$ membranes derived from PIS showed the type IV isotherm and possessed the hysteresis loop, which was associated with the mesoporous carbon structures, while the CMS membranes derived from PI showed the type I isotherm. For the molecular sieving probe, the C-SiO$_2$ membranes pyrolyzed at 550, 600, and 700$^{\circ}C$ showed the O$_2$ permeability of 924, 1076, and 367 Barrer (1 ${\times}$ 10$\^$-10/㎤(STP)cm/$\textrm{cm}^2$$.$s$.$cmHg) and O$_2$/N$_2$ selectivity of 9, 8, and 12.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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• pp.222-222
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• 2012

Metal oxide gas sensors based on semiconductor type have attracted a great deal of attention due to their low cost, flexible production and simple usability. However, most works have been focused on n-type oxides, while the characteristics of p-type oxide gas sensors have been barely studied. An investigation on p-type oxides is very important in that the use of them makes possible the novel sensors such as p-n diode and tandem devices. Monoclinic cupric oxide (CuO) is p-type semiconductor with narrow band gap (~1.2 eV). This is composed of abundant, nontoxic elements on earth, and thus low-cost, environment-friendly devices can be realized. However, gas sensing properties of neat CuO were rarely explored and the mechanism still remains unclear. In this work, the neat CuO layers with highly ordered mesoporous structures were prepared by a template-free, one-pot solution-based method using novel ink solutions, formulated with copper formate tetrahydrate, hexylamine and ethyl cellulose. The shear viscosity of the formulated solutions was 5.79 Pa s at a shear rate of 1 s-1. The solutions were coated on SiO2/Si substrates by spin-coating (ink) and calcined for 1 h at the temperature of $200{\sim}600^{\circ}C$ in air. The surface and cross-sectional morphologies of the formed CuO layers were observed by a focused ion beam scanning electron microscopy (FIB-SEM) and porosity was determined by image analysis using simple computer-programming. XRD analysis showed phase evolutions of the layers, depending on the calcination temperature, and thermal decompositions of the neat precursor and the formulated ink were investigated by TGA and DSC. As a result, the formation of the porous structures was attributed to the vaporization of ethyl cellulose contained in the solutions. Mesoporous CuO, formed with the ink solution, consisted of grains and pores with nano-meter size. All of them were strongly dependent on calcination temperature. Sensing properties toward H2 and C2H5OH gases were examined as a function of operating temperature. High and fast responses toward H2 and C2H5OH gases were discussed in terms of crystallinity, nonstoichiometry and morphological factors such as porosity, grain size and surface-to-volume ratio. To our knowledge, the responses toward H2 and C2H5OH gases of these CuO gas sensors are comparable to previously reported values.

• Bulletin of the Korean Chemical Society
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• 제20권3호
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• pp.291-296
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• 1999

The immobilization of APTMS(3-(2-aminoethylamino)propyltrimethoxysilane) and AAPTMS(3-(2-(2-aminoethyl)aminoethylanino)propyltrimethoxysilane) on the surface of high quality mesoporous molecular sieves MCM-41 and MCM-48 have been confirmed by F.T.-IR spectroscopy, Raman spectroscopy, 29Si solid state NMR, and a surface polarity measurement using Reichardt's dye. The formation of metal (Co(Ⅱ), Ni(Ⅱ), and Cu(Ⅱ)) complexes by immobilized aminosilanes have been investigated by photoacoustic spectroscopy(PAS). The assignment of UV-Vis. PAS bands makes it possible to identify the structure of metal complexes within mesoporous molecular sieves. Co(Ⅱ) ion may be coordinated mainly in a tetrahedral symmetry by two APTMS onto MCM-41, and in an octahedral one by two AAPTMS. Both Ni(Ⅱ) and Cu(Ⅱ) coordinated by aminosilanes within MCM-41 form possibly the octahedral complexes such as [Ni(APTMS)2(H20)2]2+, [Ni(AAPTMS)2]2+, [Cu(APTMS)2(H2O)2]2+, and [Cu(AAPTMS)(H2O)3]2+, respectively. The PAS band shapes of complexes onto MCM-48 are similar to those of corresponding MCM-41 with the variation of PAS intensity. Most of metal ion(Ⅱ) within MCM-41 and MCM-48 are coordinated by aminosilanes without the impregnation on the surface.

• 한국재료학회지
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• 제22권10호
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• pp.526-530
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• 2012

Silica-based ceramic-matrix composites have shown promise as advanced materials for many applications such as chemical catalysts, ceramics, pharmaceuticals, and electronics. $SiO_2$-CuO-$CeO_2$ multi-component powders and their thin film, using an oxalic acid template as a chelating agent, have larger surface areas and more uniform pore size distribution than those of inorganic acid catalysts. $SiO_2$-CuO-$CeO_2$ composite powders were synthesized using tetraethylorthosilicate, copper (II) nitrate hemi (pentahydrate), and cerium (III) nitrate hexahydrate with oxalic acid as template or pore-forming agent. The process of thermal evolution, the phase composition, and the surface morphology of these powders were monitored by thermogravimetry-differential thermal analysis (TG-DTA), X-ray diffractometry (XRD), field-emission scanning electron microscopy (FE-SEM), and energy dispersive X-ray spectrometry (EDXS). The mesoporous property of the powders was observed by Brunner-Emmett-Teller surface (BET) analysis. The improved surface area of this powder template with oxalic acid was $371.4m^2/g$. This multi-component thin film on stainless-steel was prepared by sol-gel dip coating with no cracks.