• Title/Summary/Keyword: ordered mesoporous silica

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Electrical and Mechanical Properties of Ordered Mesoporous Silica Film with HMDS Treatment

  • Ha, Tae-Jung;Choi, Sun-Gyu;Reddy, A. Sivasankar;Yu, Byoung-Gon;Park, Hyung-Ho
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.11a
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    • pp.159-159
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    • 2007
  • In order to reduce a signal delay in ULSI, low resistive metal and intermetal dielectric material of low dielectric constant are required. Ordered mesoporous silica film is proper to intermetal dielectric due to its low dielectric constant and superior mechanical properties. In this study, ordered mesoporous silica films was synthesized using TEOS (tetraethoxysilane) / MTES (methyltriethoxysilane) mixed silica precursor and Brij-$76^{(R)}$ surfactant. These films had the porosity of 40% and dielectric constant of 2.5. To lower dielectric constant, the ordered mesoporous silica films were surface-modified by HMDS (hexamethyldisilazane) treatment. HMDS substituted -OH groups on the surface of silica wall for -Si$(CH_3)_3$ groups. After the HMDS treatment, ordered mesoporous silica films were calcined at various calcination temperatures. Through the investigation, it was concluded that the proper calcination temperature is necessary as aspects of structural, electrical, and mechanical properties.

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Synthesis of Ordered Mesoporous Manganese Oxides by Double Replication for Use as an Electrode Material

  • Guo, Xiao-Feng;Kim, Geon-Joong
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.186-190
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    • 2011
  • Periodically ordered mesoporous manganese oxides were synthesized in a single and double replication procedure. Mesoporous SBA-15 and -16 silica and their reverse replica carbons were successively used as hard templates. The silica and carbon pore systems were infiltrated with $Mn(NO_3)_2{\cdot}xH_2O$ or $Mn(AcAc)_2$, which was then converted to $Mn_2O_3$ at 873 K; the silica and carbon matrix were finally removed by NaOH solution or calcinations in air. The structure of the mesoporous $Mn_2O_3$, using a carbon template, corresponds to that of the original SBA-15 and SBA-16 silica. The products consist of hexagonally arranged cylindrical mesopores with crystalline pore walls or cubic mesoporous pores. The structure of replica has been confirmed by XRD, TEM analysis, and its electrochemical properties were tested with cyclic voltammetry. Formation of $Mn_2O_3$ inside the mesoporous carbon pore system showed much improved electrical properties.

HMDS Treatment of Ordered Mesoporous Silica Film for Low Dielectric Application (저유전물질로의 응용을 휘한 규칙성 메조포러스 실리카 박막에의 HMDS 처리)

  • Ha, Tae-Jung;Choi, Sun-Gyu;Yu, Byoung-Gon;Park, Hyung-Ho
    • Journal of the Korean Ceramic Society
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    • v.45 no.1
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    • pp.48-53
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    • 2008
  • In order to reduce signal delay in ULSI, an intermetal material of low dielectric constant is required. Ordered mesoporous silica film is proper to intermetal dielectric due to its low dielectric constant and superior mechanical properties. The ordered mesoporous silica film prepared by TEOS (tetraethoxysilane) / MTES (methyltriethoxysilane) mixed silica precursor and Brij-76 surfactant was surface-modified by HMDS (hexamethyldisilazane) treatment to reduce its dielectric constant. HMDS can substitute $-Si(CH_3)_3$ groups for -OH groups on the surface of silica wall. In order to modify interior silica wall, HMDS was treated by two different processes except the conventional spin coating. One process is that film is dipped and stirred in HMDS/n-hexane solution, and the other process is that film is exposed to evaporated HMDS. Through the investigation with different HMDS treatment, it was concluded that surface modification in evaporated HMDS was more effective to modify interior silica wall of nano-sized pores.

Electrodeposition of Polypyrrole Nanowires within Vertically Oriented Mesoporous Silica Template

  • Kang, Ho-Suk;Lee, Ho-Chun;Kwak, Ju-Hyoun
    • Journal of the Korean Electrochemical Society
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    • v.14 no.1
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    • pp.22-26
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    • 2011
  • Polypyrrole (Ppy) nanowire has been electrochemically synthesized via vertically oriented mesoporous silica template. The mesoporous template is also electrochemically deposited on indium tin oxide coated (ITO) glass from tetraethyl orthosilicate (TEOS) and cetyltrimethylammonium bromide (CTAB) surfactant. The highly ordered silica template is demonstrated to be 100~120nm thick with the pores of 4~5 nm diameter by scanning electron microscope (SEM) and transmission electron microscope (TEM). Ppy is formed to fill pores of the silica template from pyrrole solution by electrochemical oxidation. The Ppy in Ppy/silica/ITO composite was found to exhibit reversible electrochemical activity, as characterized by cyclic voltammetry (CV).

Lyophobized Ordered Mesoporous Silica Additives for Li-O2 Battery Cathode

  • Roev, Victor;Ma, Sang Bok;Lee, Dong Joon;Im, Dongmin
    • Journal of Electrochemical Science and Technology
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    • v.5 no.2
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    • pp.58-64
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    • 2014
  • The surface of an ordered mesoporous silica (OMS) was functionalized using 1H,1H,2H,2H-perfluorooctyltrimethoxysilane at $20^{\circ}C$ and $60^{\circ}C$. It was shown that only elevated temperature allows lyophobic properties on the walls of OMS, eventually preventing pore flooding with nonaqueous electrolytes. The functionalized OMSs (OMS-F) were characterized with various techniques: wettability test, $N_2$ sorption measurement, high-resolution transmission electron microscopy (HR-TEM). Cathodes of $10mg/cm^2$ loading were prepared with a commercial Pt/C catalyst and polyvinylidene fluoride (PVDF, 2.5 wt.%) binder using a typical doctor blade method on a commercial gas diffusion layer (GDL) in the presence or in the absence of OMS-F additives. Subsequent discharge-charge curves were taken in a 1M LiTFSI-TEGDME electrolyte at 60oC in pure oxygen atmosphere. It was found that the discharge capacity was significantly affected by OMS-F: 5 wt.% of additive extended discharge capacity by a factor 1.5. On the other hand, a similar OMS material but synthesized at $20^{\circ}C$ did not show lyophobic properties and deteriorated cathode capacity.

Effects of Silica Shell Encapsulated Nanocrystals on Active χ-Fe5C2 Phase and Fischer-Tropsch Synthesis

  • Seunghee Cha;Heewon Kim;Hyunkyung Cho;Chul Sung Kim;Kyoung-Su Ha
    • Nanomaterials
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    • v.12 no.20
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    • pp.3704-3718
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    • 2022
  • Among various iron carbide phases, χ-Fe5C2, a highly active phase in Fischer-Tropsch synthesis, was directly synthesized using a wet-chemical route, which makes a pre-activation step unnecessary. In addition, χ-Fe5C2 nanoparticles were encapsulated with mesoporous silica for protection from deactivation. Further structural analysis showed that the protective silica shell had a partially ordered mesoporous structure with a short range. According to the XRD result, the sintering of χ-Fe5C2 crystals did not seem to be significant, which was believed to be the beneficial effect of the protective shell providing restrictive geometrical space for nanoparticles. More interestingly, the protective silica shell was also found to be effective in maintaining the phase of χ-Fe5C2 against re-oxidation and transformation to other iron carbide phases. Fischer-Tropsch activity of χ-Fe5C2 in this study was comparable to or higher than those from previous reports. In addition, CO2 selectivity was found to be very low after stabilization.

메조기공 유기실리케이트 제조에 대한 템플레이트의 영향

  • 차국헌;조은범;김상철;조휘랑
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2002.11a
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    • pp.49-49
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    • 2002
  • A strategy for the synthesis of more stable and large periodic mesoporous organo-silica materials has been developed for the 2D hexagonal mesoporous organosilica by the core-shell approach using nonionic PEO-PLGA-PEO triblock copolymer templates. The BET surface area of the solvent-extracted hexagonal mesoporous organosilica is estimated to be 1,016 ㎡/g and the pore volume, pore diameter, and wall thickness are 1.447 ㎤/g, 65 Å, and 43 Å, respectively. More hydrophobic PLGA block than the PPO block used for templates of mesoporous silica proves to be quite effective in confining the organosilicates within the PEO phase. Reaction temperature and acid concentration of an initial solution as well as the chemical nature of the bloc k copolymer templates also demonstrate to be important experimental parameters for ordered organosilica mesophase. Moreover, the mesoporous organosilicas prepared with the PEO-PLGA-PEO block templates maintain their structural integrity for up to 25 days in boiling water at 100℃. The mesoporous materials with large pores and high hydrothermal stability prepared in this study has a potential for many applications.

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Characterization and Pore Structure of Ordered Mesoporous SBA-15 Silica by Aging Condition (숙성조건 의한 메조포러스 SBA-15 실리카의 기공구조와 특성)

  • Kim, Han-Ho;Park, Hyun;Kim, Kyung-Nam
    • Korean Journal of Materials Research
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    • v.20 no.5
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    • pp.252-256
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    • 2010
  • The study was done to change the morphology and pore size of SBA-15 silica, and the characteristics of SBA-15 silica were investigated with TG-DSC, XRD, SEM, TEM and N2 adsorption-desorption under changing aging conditions. SBA-15 silica having a 2D-hexagonal structure was synthesized and confirmed by SEM and TEM. The structure of mesoporus silica SBA-15 showed a pore having regularly formed hexagonal structure and a passage having a cylindrical shape. This result is in good agreement with the pore forming in XRD and cylindrical shape of the structure in $N_2$ adsorption-desorption isotherm. SBA-15 silica showed a large BET surface area of $603-698\;m^2/g$, a pore volume of $0.673-0.926\;cm^3/g$, a large pore diameter of 5.62-7.42 nm, and a thick pore wall of 3.31-4.37 nm. This result shows that as the aging temperature increases, the BET surface area, pore volume, and pore diameter increase but the pore wall thickness decreases. The BET surface areas in SM-2 and SM-3 are as large as $698\;m^2/g$. However, SM-2 has a large surface area and forms a thick pore wall, when the aging temperature is $100^{\circ}C$ and is synthesized into stable mesoporous SBA-15 silica.

Design of Mesoporous Silica at Low Acid Concentrations in Triblock Copolymer-Butanol-Water Systems

  • Kleitz, Freddy;Kim, Tae-Wan;Ryoo, Ryong
    • Bulletin of the Korean Chemical Society
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    • v.26 no.11
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    • pp.1653-1668
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    • 2005
  • Assembly of hybrid mesophases through the combination of amphiphilic block copolymers, acting as structuredirecting agents, and silicon sources using low acid catalyst concentration regimes is a versatile strategy to produce large quantities of high-quality ordered large-pore mesoporous silicas in a very reproducible manner. Controlling structural and textural properties is proven to be straightforward at low HCl concentrations with the adjustment of synthesis gel composition and the option of adding co-structure-directing molecules. In this account, we illustrate how various types of large-pore mesoporous silica can easily be prepared in high phase purity with tailored pore dimensions and tailored level of framework interconnectivity. Silica mesophases with two-dimensional hexagonal (p6mm) and three-dimensional cubi (Fm$\overline{3}$m, Im$\overline{3}$m and Ia$\overline{3}$d) symmetries are generated in aqueous solution by employing HCl concentrations in the range of 0.1−0.5 M and polyalkylene oxide-based triblock copolymers such as Pluronic P123 $(EO_{20}-PO_{70}-EO_{20})$ and Pluronic F127 $(EO_{106}-PO_{70}-EO_{106})$. Characterizations by powder X-ray diffraction, nitrogen physisorption, and transmission electron microscopy show that the mesoporous materials all possess high specific surface areas, high pore volumes and readily tunable pore diameters in narrow distribution of sizes ranging from 4 to 12 nm. Furthermore, we discuss our recent advances achieved in order to extend widely the phase domains in which single mesostructures are formed. Emphasis is put on the first synthetic product phase diagrams obtained in $SiO_2$-triblock copolymer-BuOH-$H_2O$ systems, with tuning amounts of butanol and silica source correspondingly. It is expected that the extended phase domains will allow designed synthesis of mesoporous silicas with targeted characteristics, offering vast prospects for future applications.