• Title/Summary/Keyword: ordered mesoporous

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Preparation of Silicon-Carbon Composite via Magnesiothermic Reduction Method and Its Application to the Anode Material for Lithium Ion Battery (마그네슘열환원법을 이용한 실리콘-탄소 복합재 제조 및 리튬이차전지 음극재로의 이용)

  • Kim, Eudem;Kwon, Soon Hyung;Kim, Myung-Soo;Jung, Ji Chul
    • Korean Journal of Materials Research
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    • v.24 no.5
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    • pp.243-248
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    • 2014
  • Silicon-carbon composite was prepared by the magnesiothermic reduction of mesoporous silica and subsequent impregnation with a carbon precursor. This was applied for use as an anode material for high-performance lithium-ion batteries. Well-ordered mesoporous silica(SBA-15) was employed as a starting material for the mesoporous silicon, and sucrose was used as a carbon source. It was found that complete removal of by-products ($Mg_2Si$ and $Mg_2SiO_4$) formed by side reactions of silica and magnesium during the magnesiothermic reduction, was a crucial factor for successful formation of mesoporous silicon. Successful formation of the silicon-carbon composite was well confirmed by appropriate characterization tools (e.g., $N_2$ adsorption-desorption, small-angle X-ray scattering, X-ray diffraction, and thermogravimetric analyses). A lithium-ion battery was fabricated using the prepared silicon-carbon composite as the anode, and lithium foil as the counter-electrode. Electrochemical analysis revealed that the silicon-carbon composite showed better cycling stability than graphite, when used as the anode in the lithium-ion battery. This improvement could be due to the fact that carbon efficiently suppressed the change in volume of the silicon material caused by the charge-discharge cycle. This indicates that silicon-carbon composite, prepared via the magnesiothermic reduction and impregnation methods, could be an efficient anode material for lithium ion batteries.

Rare-Earth Metal Complex-Functionalized Mesoporous Silica for a Potential UV Sensor (잠재적인 UV 센서를 위한 희토류 금속착물이 기능화된 메조다공성 실리카)

  • Sung Soo Park;Mi-Ra Kim;Weontae Oh;Yedam Kim;Yeeun Lee;Youngeon Lee;Kangbeom Ha;Dojun Jung
    • Journal of Adhesion and Interface
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    • v.24 no.4
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    • pp.136-142
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    • 2023
  • In this study, TEOS was used as a silica source, and a triblock copolymer (P123) was used as a template to produce mesoporous silica with a well-ordered hexagonal mesopore array through a self-assembly method and hydrothermal process under acidic condition. (Surfactant-extracted SBA-15). Surfactant-extracted SBA-15 showed the particle shape of a short rod with a size of approximately 980 nm. The surface area and pore diameter were 730 m2g-1 and 70.8 Å, respectively. Meanwhile, aminosilane (3-aminopropyltriethoxysilane, APTES) was grafted into the mesopores using a post-synthesis method. Mesoporous silica (APTES-SBA-15) modified with aminosilane had a well-ordered pore structure (p6mm) and well-maintained the particle shape of short rods. The surface area and pore diameter of APTES-SBA-15 decreased to 350 m2g-1 and 60.7 Å, respectively. APTES-modified mesoporous silica was treated with a solution of rare earth metal ions (Eu3+, Tb3+) to synthesize a mesoporous silica material in which rare earth metal complexes were introduced into the mesopores. (Eu/APTES-SBA-15, Tb/APTES-SBA-15) These materials exhibited characteristic photoluminescence spectra by λex=250 nm. (5D47F5 (543.5 nm), 5D47F4 (583.5 nm), 5D47F3 (620.2 nm) transitions for Tb/APTES-SBA-15; 5D07F0 (577.7 nm), 5D07F1 (592.0 nm), 5D07F2 (614.9 nm), 5D07F3 (650.3 nm) and 5D07F4 (698.5 nm) transitions for Eu/APTES-SBA-15)

Soft-template Synthesis of Magnetically Separable Mesoporous Carbon (자성에 의해 분리 가능한 메조포러스 카본의 소프트 주형 합성)

  • Park, Sung Soo;Ha, Chang-Sik
    • Journal of Adhesion and Interface
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    • v.18 no.2
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    • pp.75-81
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    • 2017
  • In this study, we synthesized mesoporous carbon (Carbonized Ni-FDU-15) containing nanoporous structures and magnetic nanoparticles. Carbonized Ni-FDU-15 was synthesized via evaporation-induced self-assembly (EISA) and direct carbonization by using a triblock copolymer (F127) as a structure-directing agent, a resol precursor as a carbon-pore wall forming material, and nickel (II) nitrate as a metal ion source. The mesoporous carbon has a well-ordered two-dimensional hexagonal structure. Meanwhile, nickel (Ni) metal and nickel oxide (NiO) were produced in the magnetic nanoparticles in the pore wall. The size of the nanoparticles was about 37 nm. The surface area, pore size and pore volume of Carbonized Ni-FDU-15 were $558m^2g^{-1}$, $22.5{\AA}$ and $0.5cm^3g^{-1}$, respectively. Carbonized Ni-FDU-15 was found to move in the direction of magnetic force when magnetic force was externally applied. The magnetic nanoparticle-bearing mesoporous carbons are expected to have high applicability in a wide variety of applications such as adsorption/separation, magnetic storage media, ferrofluid, magnetic resonance imaging (MRI) and drug targeting, etc.

Synthesis and Characterization of Cu2+-Perfluorophthalocyanine Incorporated SBA15

  • Oh, Mi-Ok;Park, Sung Soo;Ha, Chang-Sik
    • Journal of Adhesion and Interface
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    • v.7 no.3
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    • pp.10-15
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    • 2006
  • After anchoring 3-(2-aminoethylamino)propyltriethoxysilane (APTES) onto the surfaces of the channels within ordered mesoporous silica, SBA-15, we dispersed $Cu^{2+}$-perfluorophthalocyanine into the modified SBA-15 channels. From small-angle X-ray scattering (SAXS) patterns and transmission electron microscopy (TEM) images, we confirmed that both the calcined and $Cu^{2+}$-perfluorophthalocyanine-incorporated SBA-15 samples possessed ordered periodic structures and hexagonal symmetry lattices (p6mm). The value of the $d_{100}$ spacing was decreased after the incorporation of $Cu^{2+}$-perfluorophthalocyanine into the modified SBA-15 channels. We used FTIR and UV-Vis spectroscopy and thermogravimetric analysis (TGA) to characterize both the modified SBA-15 and the $Cu^{2+}$-perfluorophthalocyanine-incorporated SBA-15 samples. From scanning electron microscopy (SEM) images and $N_2$ sorption measurements, we found that the $Cu^{2+}$-perfluorophthalocyanine units were incorporated within the modified SBA-15 channels, rather than on the external surfaces of the modified SBA-15 channels.

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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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Interfacial Layer Control in DSSC

  • Lee, Wan-In
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.75-75
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    • 2011
  • Recently, dye-sensitized solar cell (DSSC) attracts great attention as a promising alternative to conventional silicon solar cells. One of the key components for the DSSC would be the nanocrystalline TiO2 electrode, and the control of interface between TiO2 and TCO is a highly important issue in improving the photovoltaic conversion efficiency. In this work, we applied various interfacial layers, and analyzed their effect in enhancing photovoltaic properties. In overall, introduction of interfacial layers increased both the Voc and Jsc, since the back-reaction of electrons from TCO to electrolyte could be blocked. First, several metal oxides with different band gaps and positions were employed as interfacial layer. SnO2, TiO2, and ZrO2 nanoparticles in the size of 3-5 nm have been synthesized. Among them, the interfacial layer of SnO2, which has lower flat-band potential than that of TiO2, exhibited the best performance in increasing the photovoltaic efficiency of DSSC. Second, long-range ordered cubic mesoporous TiO2 films, prepared by using triblock copolymer-templated sol-gel method via evaporation-induced self-assembly (EISA) process, were utilized as an interfacial layer. Mesoporous TiO2 films seem to be one of the best interfacial layers, due to their additional effect, improving the adhesion to TCO and showing an anti-reflective effect. Third, we handled the issues related to the optimum thickness of interfacial layers. It was also found that in fabricating DSSC at low temperature, the role of interfacial layer turned out to be a lot more important. The self-assembled interfacial layer fabricated at room temperature leads to the efficient transport of photo-injected electrons from TiO2 to TCO, as well as blocking the back-reaction from TCO to I3-. As a result, fill factor (FF) was remarkably increased, as well as increase in Voc and Jsc.

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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.

Photochromic Spiropyran-Functionalized Organic-Inorganic Hybrid Mesoporous Silica for Optochemical Gas Sensing (광화학적 가스 센싱을 위한 광변색 스피로피란 개질된 유기-무기 하이브리드 메조포러스 실리카)

  • Park, Sung Soo;Ha, Chang-Sik
    • Journal of Adhesion and Interface
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    • v.17 no.4
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    • pp.141-148
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    • 2016
  • In this work, mesoporous silica (SBA-15) was synthesized via self-assembly process using triblock copolymer ($PEO_{20}PPO_{70}PEO_{20}$, P123) as template and tetraethyl orthosilicate (TEOS) as silica source under acidic condition. SBA-15 have high surface area ($704m^2g^{-1}$) and uniform pore size (8.4 nm) with well-ordered hexagonal mesostructure. Spiropyran-functionalized SBA-15 (Spiropyran-SBA-15) was synthesized via post-synthesis process using 3-(triethoxysilyl)propyl isocyanate (TESPI) and 1-(2-Hydroxyethyl)-3,3-dimethy-lindolino-6'-nitrobenzopyrylo-spiran (HDINS). Spiropyran-SBA-15 was produced with hexagonal array of mesopores without damage of mesostructre. Surface area and pore size of Spiropyran-SBA-15 were $651m^2g^{-1}$ and 8.0 nm, respectively. Optochemical properties of Spiropyran-SBA-15 was studied with chemical vapors such as EtOH, THF, $CHCl_3$, Acetone and HCl. Main peaks of photofluorescence of Spiropyran-SBA-15 exhibited blue shift in the range of 603.4~592.1 nm after exposure under EtOH, THF, $CHCl_3$, and Acetone vapors. Normalized peak intensities decreased in the range of 0.8~0.3. The main peak of photofluorescence of Spiropyran-SBA-15 showed significant blue shift of 592.1 nm after exposure under HCl vapor, while normalized peak intensity decreased to 0.1.