• Title/Summary/Keyword: Mesoporous $SiO_2$

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Fabrication and Characterization of Macro/Mesoporous SiC Ceramics from SiO2 Templates (실리카 주형을 이용한 메크로/메조다공성 탄화규소 세라믹의 제조와 비교특성)

  • ;Hao Wang
    • Journal of the Korean Ceramic Society
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    • v.41 no.7
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    • pp.528-533
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    • 2004
  • Macroporous SiC with pore size 84∼658 nm and mesoporous SiC with pore size 15∼65 nm were respectively prepared by infiltrating low viscosity preceramic polymer solutions into the various sacrificial templates obtained by natural sedimentation or centrifuge of 20∼700 nm silica sol, which were subsequently etched off with HF after pyrolysis at 1000∼140$0^{\circ}C$ in an argon atmosphere. Three-dimensionally long range ordered macroporous SiC ceramics derived from polymethylsilane (PMS) showed surface area 584.64$m^2$g$^{-1}$ when prepared with 112nm silica sol and at 140$0^{\circ}C$, whereas mesoporous SiC from polycarbosilane (PCS) exhibited the highest surface area 619.4 $m^2$g$^{-1}$ with random pore array when prepared with 20-30 nm silica sol and at 100$0^{\circ}C$. Finally, tile pore characteristics of porous SiC on the types of silica sol, polymers and pyrolytic conditions were interpreted with the analytical results of SEM, TEM, and BET instruments.

Characteristics of p-Xylene Adsorption using Functionalized Mesoporous Silica (관능기화 메조포러스 실리카를 이용한 파라자일렌 흡착 특성)

  • Kim, Sang-Hyoun;Park, Jonghoon;Kang, Seok-Tae;Chung, Jae-Woo;Kim, Soo-Hong;Cho, Yunchul;Lee, Chae-Young
    • Journal of the Korean GEO-environmental Society
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    • v.13 no.6
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    • pp.27-31
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    • 2012
  • This study was designed to examine the feasibility of functionalized mesoporous silica as the adsorbent for benzene, toluene, ethylbenzene, and xylene isomers (BTEX) in groundwater. p-Xylene was used as the model compound of BTEX. A series of functionalized mesoporous silica with MCM-41 type of structure was synthesized using a co-condensation method. Monoamine, triamine, nitrile, phenyl, and octyl groups were functionalized to the mesoporous silica structure. Adsorption sites for p-Xylene in a functionalized mesoporous silica were Si-O-Si covalent bond, the surfactant, and the functional group. Octyl-functionalized mesoporous silica with stearyltrimethylammonium chloride as a surfactant showed the highest adsorption ability. The maximum xylene adsorption capacity of the octyl-functionalized mesoporous silica with stearyltrimethylammonium chloride based on Langmuir model was 4.17 mmol/g on $20^{\circ}C$, which was 2.9 times higher than that of MCM-41.

Template Synthesis of Ordered-Mesoporous Tin Oxide for Lithium-ion Battery Anode Materials (주형 합성법을 통해 합성된 다공성 주석 산화물을 적용한 리튬이차전지용 음극재 연구)

  • Seo, Gyeongju;Choi, Jaecheol;Lee, Yong Min;Ko, Chang Hyun
    • Journal of the Korean Electrochemical Society
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    • v.17 no.2
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    • pp.86-93
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    • 2014
  • Mesoporous tin oxide (meso-$SnO_2$) with 5 nm mesopore and well-aligned $SnO_2$ nanowire-bundles with 5~7 nm diameters were prepared by template synthesis method. In addition to meso-$SnO_2$, meso-$SnO_2$/$SiO_2$, which has almost the same structure as meso-$SnO_2$ including $SiO_2$ used as the template were prepared by the modification of template synthesis. X-ray diffraction, N2 adsorption-desorption isotherms, transmission electron microscopy observed structures of meso-$SnO_2$ and meso-$SnO_2$/$SiO_2$. Although the meso-$SnO_2$/$SiO_2$ showed some positive evidences to suppress the volume change of meso-$SnO_2$ through cyclic voltammogram, electrochemical impedance spectroscopy, and voltage profiles during cycling, its cycle life was not improved highly to address modified structural effects. Thus, further study might be done to control the nanostructure of meso-$SnO_2$/$SiO_2$ for enhanced cycle performance.

Confined Pt and CoFe2O4 Nanoparticles in a Mesoporous Core/Shell Silica Microsphere and Their Catalytic Activity

  • Kang, Dong-Hyeon;Eum, Min-Sik;Lee, Byeong-No;Bae, Tae-Sung;Lee, Kyu-Reon;Lim, Heung-Bin;Hur, Nam-Hwi
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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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.

Derivation of Cubic and Hexagonal Mesoporous Silica Films by Spin-coating

  • Pan, Jia-Hong;Lee, Wan-In
    • Bulletin of the Korean Chemical Society
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    • v.26 no.3
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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.

Microwave Synthesis of Titanium Silicalite-1 Using Solid Phase Precursors

  • Kim, K.Y.;Ahn, W.S.;Park, D.W.;Oh, J.H.;Lee, C.M.;Tai, W.P.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.5
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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.

Fabrication of High Permeable Nanoporous Carbon-SiO$_2$ Membranes Derived from Siloxane-containing Polyimides

  • Kim, Youn Kook;Han, Sang Hoon;Park, Ho Bum;Lee, Young Moo
    • Korean Membrane Journal
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    • v.6 no.1
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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.

Hydrogen and Ethanol Gas Sensing Properties of Mesoporous P-Type CuO

  • Choi, Yun-Hyuk;Han, Hyun-Soo;Shin, Sun;Shin, Seong-Sik;Hong, Kug-Sun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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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.

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The Formation of Metal (M=Co(II), Ni(II), and Cu(II)) Complexes by Aminosilanes Immobilized within Mesoporous Molecular Sieves

  • 박동호;박성수;최상준
    • Bulletin of the Korean Chemical Society
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    • v.20 no.3
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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.

Preparation of SiO2-CuO-CeO2 Composite Powders and Its Thin Film Templated with Oxalic Acid

  • Son, Boyoung;Jung, Miewon
    • Korean Journal of Materials Research
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    • v.22 no.10
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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.