• Title/Summary/Keyword: Template-free synthesis

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Preparation of Mesoporous Titanium Oxides by Template Synthesis and Phase Transition of TiO2 inside Mesoporous Silica (주형합성을 통한 메조포러스 TiO2 제조 및 실리카 메조포어 내부에서의 TiO2 상전이 거동 변화)

  • Bang, Gyeong-Min;Kim, Young-Ji;Kim, Seung Han;Choi, Yerak;Lee, In Ho;Ko, Chang Hyun
    • Korean Chemical Engineering Research
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    • v.56 no.2
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    • pp.261-268
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    • 2018
  • To prepare mesoporous $TiO_2$ ($meso-TiO_2$) with anatase and rutile crystal structures, hydrothermal and template synthesis were used. $Meso-TiO_2$ with anatase structure was obtained by hydrothermal synthesis. The crystal structure of $meso-TiO_2$ by hydrothermal synthesis converted from anatase to rutile by simple heating at $600^{\circ}C$ and above. However, their mesopore structure collapsed due to phase transition. To prepare $meso-TiO_2$ with rutile structure, template synthesis method was applied using mesoporous silica KIT-6 as a template. Once we incorporated anatase $TiO_2$ inside mesopores of silica, the phase transition temperature of $TiO_2$ confined inside KIT-6 was much higher ($900^{\circ}C$) than that of free-standing $TiO_2$ ($600^{\circ}C$). The suppression of $TiO_2$ phase transition inside mesopores of KIT-6 is closely related with the interaction between $TiO_2$ surface and silica walls in KIT-6 because oxygen vacancy in $TiO_2$ is regarded as the starting point for phase transition. After removal of silica template by NaOH solution washing, $meso-TiO_2$ with mixed phase between anatase and rutile was obtained.

Three-dimensional porous graphene materials for environmental applications

  • Rethinasabapathy, Muruganantham;Kang, Sung-Min;Jang, Sung-Chan;Huh, Yun Suk
    • Carbon letters
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    • v.22
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    • pp.1-13
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    • 2017
  • Porous materials play a vital role in science and technology. The ability to control their pore structures at the atomic, molecular, and nanometer scales enable interactions with atoms, ions and molecules to occur throughout the bulk of the material, for practical applications. Three-dimensional (3D) porous carbon-based materials (e.g., graphene aerogels/hydrogels, sponges and foams) made of graphene or graphene oxide-based networks have attracted considerable attention because they offer low density, high porosity, large surface area, excellent electrical conductivity and stable mechanical properties. Water pollution and associated environmental issues have become a hot topic in recent years. Rapid industrialization has led to a massive increase in the amount of wastewater that industries discharge into the environment. Water pollution is caused by oil spills, heavy metals, dyes, and organic compounds released by industry, as well as via unpredictable accidents. In addition, water pollution is also caused by radionuclides released by nuclear disasters or leakage. This review presents an overview of the state-of-the-art synthesis methodologies of 3D porous graphene materials and highlights their synthesis for environmental applications. The various synthetic methods used to prepare these 3D materials are discussed, particularly template-free self-assembly methods, and template-directed methods. Some key results are summarized, where 3D graphene materials have been used for the adsorption of dyes, heavy metals, and radioactive materials from polluted environments.

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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Synthesis of Hollow Silica Using PMMA Particle as a Template (PMMA 고분자 입자를 템플릿으로 이용한 실리카 중공체의 제조)

  • Hwang, Ha-Soo;Cho, Kye-Min;Park, In
    • Applied Chemistry for Engineering
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    • v.21 no.3
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    • pp.353-355
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    • 2010
  • Poly(methyl methacrylate) (PMMA) particles were prepared by soap-free emulsion polymerization of MMA in the presence of a cationic initiator, 2,2'-azobis(2-methylpropionamidine) (AIBA). The Stober method has been adopted to coat silica on the surface of these cationic particles. Negatively charged silica precursors were coated onto cationic particle surfaces by electronic interaction. During the coating process, hollow particles were directly obtained by dissolution of PMMA.

Composite Materials with MWCNTs and Conducting Polymer Nanorods and their Application as Supercapacitors

  • Liua, Lichun;Yoo, Sang-Hoon;Park, Sung-Ho
    • Journal of Electrochemical Science and Technology
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    • v.1 no.1
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    • pp.25-30
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    • 2010
  • This study demonstrated the synthesis of high-surface-area metal-free carbonaceous electrodes (CE) from anodic aluminum oxide (AAO) templates, and their application as supercapacitors. Multi-walled Carbon nanotubes (MWCNTs) were interwoven into a porous network sheet that was attached to one side of AAO template through a vacuum filtration of the homogeneously dispersed MWCNT toluene solution. Subsequently, the conducting polymer was electrochemically grown into the porous MWCNT network and nanochannels of AAO, leading to the formation of a carbonaceous metal-free film electrode with a high surface area in the given geometrical surface area. Typical conducting polymers such as polypyrrole (PPY) and poly(3,4-ethylenedioxythiophene) (PEDOT) were examined as model systems, and the resulting electrodes were investigated as supercapacitors (SCs). These SCs exhibited stable, high capacitances, with values as high as 554 F/g, 1.08 F/$cm^2$ for PPY and 237 F/g, 0.98 F/$cm^2$ for PEDOT, that were normalized by both the mass and geometric area.

스퍼터링 방법으로 성장시킨 나노구조의 Ga 농도 변화에 따른 형상 변화

  • Kim, Yeong-Lee;U, Chang-Ho;Jo, Hyeong-Gyun
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2009.11a
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    • pp.23.1-23.1
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    • 2009
  • ZnO is of great interest for various technological applications ranging from optoelectronics to chemical sensors because of its superior emission, electronic, and chemical properties. In addition, vertically well-aligned ZnO nanorods on large areas with good optical and structural properties are of special interest for the fabrication of electronic and optical nanodevices. To date, several approaches have been proposed for the growth of one-dimensional (1D) ZnO nanostructunres. Several groups have been reported the MOCVD growth of ZnO nanorods with no metal catalysts at $400^{\circ}C$, and fabricated a well-aligned ZnO nanorod array on a PLD prepared ZnO film by using a catalyst-free method. It has been suggested that the synthesis of ZnO nanowires using a template-less/surfactant-free aqueous method. However, despite being a well-established and cost-effective method of thin film deposition, the use of magnetrons puttering to grow ZnO nanorods has not been reported yet. Additionally,magnetron sputtering has the dvantage of producing highly oriented ZnO film sat a relatively low process temperature. Currently, more effort has been concentrated on the synthesis of 1D ZnO nanostructures doped with various metal elements (Al, In, Ga, etc.) to obtain nanostructures with high quality,improved emission properties, and high conductance in functional oxide semiconductors. Among these dopants, Ga-doped ZnO has demonstrated substantial advantages over Al-doped ZnO, including greater resistant to oxidation. Since the covalent bond length of Ga-O ($1.92\;{\AA}$) is nearly equal to that of Zn-O ($1.97\;{\AA}$), high electron mobility and low electrical resistivity are also expected in the Ga-doped ZnO. In this article, we report the successful growth of Ga-doped ZnO nanorods on c-Sapphire substrate without metal catalysts by magnetrons puttering and our investigations of their structural, optical, and field emission properties.

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Synthesis and enhancements of exciton-phonon interactions for ZnO nanopencils by thermal evaporation (ZnO nanopencils의 합성과 향상된 exciton-phonon interactions)

  • Ahn, C.H.;Woo, C.H.;Bae, Y.S.;Choi, M.K.;Kim, Y.Y.;Kim, D.C.;Kong, B.H.;Cho, H.K.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2009.06a
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    • pp.45-45
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    • 2009
  • 우리는 ZnO Template를 사용한 열기상법을 이용하여 수직 배양한 ZnO nanorods와 ZnO Nanopencils를 성장하였고, Dependency temperature Photoluminescence(PL)의 분석을 통하여 광학적 특성에 대해 분석을 하였다. ZnO 나노구조는 100K 이하의 온도에서 donor-bound exciton가 dominant하고, 100K 이상의 온도에서는 free exciton과 그들의 phonon-replica emission이 dominant한 것을 알 수 있었다. 하지만, ZnO nanorods와 nanopencils은 다른 exciton-phonon coupling의 strength에 의한 surface defects에 의해 excitonic emissions의 다른 거동을 보이는 것을 알았다. 이것으로 인해 상온 PL에서 ZnO nanopencil은 nanorods에 비해 52meV의 red shift를 보였다.

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A Kinetic Study on the Synthesis of Dimethylcarbonate by Using Immobilized Ionic Liquid Catalyst (고정화된 이온성 액체 촉매를 이용한 디메틸카보네이트 합성 반응에 대한 속도론적 고찰)

  • Kim, Dong-Woo;Kim, Dong-Kyu;Kim, Cheol-Woong;Koh, Jae-Cheon;Park, DaeWon
    • Korean Chemical Engineering Research
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    • v.48 no.3
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    • pp.332-336
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    • 2010
  • Ionic liquid immobilized on mesoporous amorphous silica was prepared from the coupling of 1-(triethoxysilylpropyl)-3-n-alkyl-imidzolium halides with tetraethyl orthosilicate(TEOS) through template-free condensation under strong acidic conditions. The immobilized 1-n-butyl-3-methyl imidazolium bromide ionic liquid on amorphous silica(BMImBr-AS) was proved to be an effective heterogeneous catalyst for the synthesis of dimethyl carbonate(DMC) from transesterification of ethylene carbonate(EC) with methanol. High temperature, high carbon dioxide pressure and long reaction time were favorable for the reactivity of BMImBr-AS. Kinetic studies based on two step reactions revealed that the proposed reaction model fitted well the experimental data. The apparent activation energy was estimated to be 67.4 kJ/mol.

Chiral Mesoporous Silica for Asymmetric Metal-free Catalysis: Enhancement of Chirality thorough Confinement Space by Plug Effect

  • Jeong, Eun-Yeong;Im, Cheong-Rae;Park, Sang-Eon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.199-199
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    • 2011
  • The addition of a carbanion to ${\yen}{\acute{a}}{\yen}{\hat{a}}$-unsaturated carbonyl compounds is of importance in the C-C bond formation reactions for modern pharmaceuticals and organic synthesis. Recently, heterogeneous asymmetric catalysis became more attractive area of research because of the easy recovery and separation of the catalyst from the reaction system. Most of synthetic methods for heterogeneous catalysts were grafting or immobilization of homogeneous catalyst onto the solid supports. Trans-1,2-Diaminocyclohexane(DACH) and L-proline ligands have been enormously used as chiral ligands in several catalytic transformation under homogenous conditions. Our group prepared l-proline functionalized mesoporous silica was synthesized under acidic condition using a poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer template (EO20PO70EO20, Pluronic P-123, BASF). Furthermore, we successfully directly synthesized trans-1,2 diaminocyclohexane functionalized mesoporous silica by using microwave method. The direct functionalization of chiral ligand into the framework of mesoporous materials is expected to be useful for the heterogeneous asymmetric catalysis. So, we adopt the direct synthesis of chiral ligand functionalized mesoporous silica by using thermal and microwave irradiation. Then, chiral ligand functionalized mesoporous silicas were applied to enantioselective asymmetric catalytic reactions.

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Use of Core-Crosslinked Amphiphilic Polymer Nanoparticles as Templates for Synthesis of Nanostructured Inorganic Materials (코아 가교 양친성 고분자 나노입자 템플레이트를 이용한 무기물 나노 구조체 합성)

  • Kim, Hyun-Ji;Kim, Na-Hae;Kim, Juyoung
    • Journal of Adhesion and Interface
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    • v.16 no.1
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    • pp.6-14
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    • 2015
  • In this study, physically and chemically stable core-crosslinked amphiphilic polymer (CCAP) nanoparticles were prepared using amphiphilic reactive precursors via soap-free emulsion process. Obtained CCAP nanoparticles were used as templates for synthesis of nanostructured $TiO_2$ nanoparticles. First, CCAP nanoparticles dispersed aqueous solutions were mixed with titanium isopropoxide to prepare stable organic-inorganic hybrid sols, and then obtained sols were spin coated onto glass substrate to prepare hybrid thin films onto glass, and then hybrid thin films were calcinated at various temperature to remove CCAP. Nanostructure of calcinated thin fims were examined by SEM. To study effect of CCAP nanoparticles on nanostructure of $TiO_2$ nanoparticles, the morphology of $TiO_2$ nanoparticles prepared using various CCAP templates was compared with that of $TiO_2$ nanoparticles prepared using conventional organic template, nonionic surfactant, Triton X-100.