• Title/Summary/Keyword: X-ray microscopy

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Preparation of Al@Fe2O3 Core-Shell Composites Using Amphiphilic Graft Copolymer Template

  • Patel, Rajkumar;Kim, Sang Jin;Kim, Jin Kyu;Park, Jung Su;Kim, Jong Hak
    • Korean Chemical Engineering Research
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    • v.52 no.2
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    • pp.209-213
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    • 2014
  • A graft copolymer of poly(vinyl chloride)-g-poly(oxyethylene methacrylate) (PVC-g-POEM) was synthesized via atom transfer radical polymerization (ATRP) and used as a structure-directing agent to prepare $Al@Fe_2O_3$ core-shell nanocomposites through a sol-gel process. The amphiphilic property of PVC-g-POEM allows for good dispersion of Al particles and leads to specific interaction with iron ethoxide, a precursor of $Fe_2O_3$. Secondary bonding interaction in the sol-gel composites was characterized by Fourier transform-infrared (FT-IR) spectroscopy. The well-organized morphology of $Al@Fe_2O_3$ core-shell nanocomposites was observed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Energy dispersive X-ray (EDX) and X-ray diffraction (XRD) were used to analyze the elemental composition and crystallization structure of the composites.

Synthesis of Cobalt Phosphates and their Catalytic Properties of the Hydrogen Generation from the Hydrolysis of NaBH4 (비결정질 코발트 인산염 합성 및 NaBH4 가수분해를 통한 수소발생 촉매 활성 연구)

  • Kim, Youngyong;Park, Joon Bum;Kwon, Ki-Young
    • Applied Chemistry for Engineering
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    • v.26 no.6
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    • pp.743-745
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    • 2015
  • Amorphous cobalt phosphates were synthesized with their distinct morphology by controlling the amount of base in the synthetic condition. The crystallinity and morphology of cobalt phosphates were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The prepared cobalt phosphates were applied as a heterogeneous catalyst for generating hydrogen gas from the hydrolysis reaction of sodium borohydride. We found that the catalyst prepared using the least amount of base condition at room temperature showed a plate shape with less than 10 nm thickness, which resulted in the best catalytic activity among all catalysts due to the large surface area.

Synthesis of Praseodymium-Doped TiO2 Nanocatalysts by Sol-Microwave and Their Photocatalytic Activity Study

  • Huang, Fengping;Wang, Shuai;Zhang, Shuang;Fan, Yingge;Li, Chunxue;Wang, Chuang;Liu, Chun
    • Bulletin of the Korean Chemical Society
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    • v.35 no.8
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    • pp.2512-2518
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    • 2014
  • The praseodymium-doped $TiO_2$ photocatalyst samples, which could degrade methyl orange under UV irradiation, were prepared by sol-microwave method for improving the photocatalytic activity of $TiO_2$. The resulting materials were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Raman spectra, Fourier transform infrared spectra (FTIR) and Ultraviolet-visible diffuse reflectance spectra (UV-vis DRS). It was found Pr doping retarded the growth of crystalline size and the phase transformation from anatase to rutile, and narrowed the band gap energy. Praseodymium doping brought about remarkable improvement in the photoactivity. The optimal dopant amount of Pr was 2% by molar of cement and the calcination temperature was $500^{\circ}C$ for the best photocatalytic activity. The improvement of photocatalytic activity was ascribed to the occurrence of lattice distortion and the effective containment of the recombination of the electron-hole by $Pr^{3+}$.

A Study of the Crystal Structure of the Fine S-Phase Precipitate in Al-Cu-Mg Alloy by Electron Diffraction Experiments (전자회절실험에 의한 알루미늄 합금 (Al-Cu-Mg)의 미세 S-상 석출입자에 대한 결정구조 연구)

  • Kim, Hwang-Su
    • Applied Microscopy
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    • v.35 no.4
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    • pp.1-9
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    • 2005
  • In this paper it is reported that a comprehensive study of the crystal structure of the fine size S-phase ($Al_2CuMg$) precipitate in Al-Cu-Mg alloy by electron diffraction experiments. The experiments involve taking the selected area diffraction pattern for a S-phase particle, simulations of the pattern based on the kinematical diffraction theory and quantitative data collection from the zone axis diffraction patterns for the comparison with calculated diffraction intensity using both the kinematical and the dynamical diffraction theory. As a result, a good fitting model of the S-phase structure turns out to be the model reported early by X-ray methods (Perlitz & Westgren, 1943), not the new model determined by HRTEM methods (Radmilovic et al., 1999).

Fabrication of ZnO Nanostructures with Various Growth Conditions by Vapor Phase Transport

  • Kim, So-A-Ram;Nam, Gi-Woong;Kim, Min-Su;Yim, Kwang-Gug;Kim, Do-Yeob; Leem, Jae-Youn
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.250-250
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    • 2011
  • Zinc oxide (ZnO) structures have great potential in many applications. Currently, the most commonly used method to grow ZnO nanostructres are the vapor transport method (VPT). The morphology of the ZnO structures largely related to the growth conditions, including growth temperature, distance between the substrate and source, and gas ambient. Previously ZnO nanosturecutres with high crystallinity were obtained at the growth temperature of 800$^{\circ}C$, in the argon and oxygen gas ambient. In this study, we report the properties of the ZnO nanostructures, which were synthesized on Au-catalyzed Si substrate by VPT, using a mixture of ZnO and graphite powders as source material under the different condition, including gas ratio of argon/oxygen and distance between substrate and source at the growth temperature of 800$^{\circ}C$. The structural and optical properties of the ZnO nanostructures were investigated by field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and photoluminescence (PL).

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Pt Electrocatalysts Composited on Electro-Spun Pt Nanowires for Direct Methanol Fuel Cells

  • An, Geon-Hyoung;Ahn, Hyo-Jin
    • Korean Journal of Materials Research
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    • v.22 no.8
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    • pp.421-425
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    • 2012
  • Two types of Pt nanoparticle electrocatalysts were composited on Pt nanowires by a combination of an electrospinning method and an impregnation method with NaBH4 as a reducing agent. The structural properties and electrocatalytic activities for methanol electro-oxidation in direct methanol fuel cells were investigated by means of scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry. In particular, SEM, HRTEM, XRD, and XPS results indicate that the metallic Pt nanoparticles with polycrystalline property are uniformly decorated on the electro-spun Pt nanowires. In order to investigate the catalytic activity of the Pt nanoparticles decorated on the electro-spun Pt nanowires, two types of 20 wt% Pt nanoparticles and 40 wt% Pt nanoparticles decorated on the electro-spun Pt nanowires were fabricated. In addition, for comparison, single Pt nanowires were fabricated via an electrospinning method without an impregnation method. As a result, the cyclic voltammetry and chronoamperometry results demonstrate that the electrode containing 40 wt% Pt nanoparticles exhibits the best catalytic activity for methanol electro-oxidation and the highest electrochemical stability among the single Pt nanowires, the 20 wt% Pt nanoparticles decorated with Pt nanowires, and the 40 wt% Pt nanoparticles decorated with Pt nanowires studied for use in direct methanol fuel cells.

The Effect of $Y_2O_3$ Addition on the Mechanical Alloying of $Ni_3$Al ($Ni_3$Al의 기계적합금화에 미치는 $Y_2O_3$ 첨가의 영향)

  • 이상태
    • Journal of Powder Materials
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    • v.4 no.3
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    • pp.205-213
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    • 1997
  • Mechanical alloying of $Ni_3Al$ and $Y_2O_3$ added ODS $Ni_3Al$ from elemental powders was investigated by the X-ray diffraction, differential scanning calorimeter, transmission electron microscopy and optical microscopy. The steady states of $Ni_3Al$ and ODS $Ni_3Al$ powders were reached after mechanical alloying with the condition of the ball-to-powder input ratio of 20:1 for 20 hours and 10 hours, respectively. The addition of nano-sized $Y_2O_3$ particles enhanced cold working and fracture, and subsequently accelerated MA of $Ni_3Al$ powders. DSC results of MAed $Ni_3Al$ powders showed four exothermic peaks at 14$0^{\circ}C$, 234$^{\circ}C$, 337$^{\circ}C$ and 385$^{\circ}C$. From the high temperature X-ray diffraction analysis, it was concluded that the peaks were resulted from the recovery solution of unalloyed Al in Ni, the formation of intermediate phase NiAl, and $LI_2$ ordering of MAed $Ni_3Al$ powders.

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Synthesis and Characterization of ZnS and ZnS/TiO2 Nanocomposites and Their Enhanced Photo-decolorization of MB and 1,5-Diphenyl Carbazide

  • Meng, Ze-Da;Ullah, Kefayat;Zhu, Lei;Ye, Shu;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.51 no.4
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    • pp.307-311
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    • 2014
  • ZnS and $ZnS/TiO_2$ were prepared by chemical deposition. The prepared photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and transmission electron microscopy (TEM). The generation of reactive oxygen species was detected by monitoring the oxidation reaction from 1,5-diphenyl carbazide (DPCI) to 1,5-diphenyl carbazone (DPCO). Excellent catalytic degradation of methylene blue (MB) solution was observed using the $ZnS/TiO_2$ composites during irradiation with visible light. The results show that the photocatalytic performance of $TiO_2$ nanoparticles is improved by loading with ZnS.

Preparation of ZnO2 Nanoparticles Using Organometallic Zinc(II) Isobutylcarbamate in Organic Solvent

  • Kim, Kyung-A;Cha, Jae-Ryung;Gong, Myoung-Seon;Kim, Jong-Gyu
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.431-435
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    • 2014
  • Zinc peroxide nanoparticles ($ZnO_2$ NPs) were prepared by reacting zinc(II) isobutylcarbamate, as an organometallic precursor, with hydrogen peroxide ($H_2O_2$) at $60^{\circ}C$. Polyethylene glycol and polyvinylpyrrolidone were used as stabilizers, which suppressed aggregation of the $ZnO_2$ NPs. Conditions such as concentrations of $H_2O_2$ and the stabilizer were systemically controlled to determine their effect on the formation of nano-sized $ZnO_2$ NPs. The formation of stable $ZnO_2$ NPs was confirmed by UV-vis, Raman spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction. The TEM images revealed that polyvinylpyrrolidone-stabilized $ZnO_2$ NPs (diameter, 10-30 nm) were well dispersed in the organic solvent. Quite pure ZnO NPs were obtained from the peroxide powder by simple heat treatment of $ZnO_2$. The transition temperature of $170^{\circ}C$ was determined by differential scanning calorimetry.

Heteroepitaxial Growth of Single 3C-SiC Thin Films on Si (100) Substrates Using a Single-Source Precursor of Hexamethyldisilane by APCVD

  • Chung, Gwiy-Sang;Kim, Kang-San
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.533-537
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    • 2007
  • This paper describes the heteroepitaxial growth of single-crystalline 3C-SiC (cubic silicon carbide) thin films on Si (100) wafers by atmospheric pressure chemical vapor deposition (APCVD) at 1350 oC for micro/nanoelectromechanical system (M/NEMS) applications, in which hexamethyldisilane (HMDS, Si2(CH3)6) was used as a safe organosilane single-source precursor. The HMDS flow rate was 0.5 sccm and the H2 carrier gas flow rate was 2.5 slm. The HMDS flow rate was important in obtaing a mirror-like crystalline surface. The growth rate of the 3C-SiC film in this work was 4.3 μm/h. A 3C-SiC epitaxial film grown on the Si (100) substrate was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), reflection high energy electron diffraction (RHEED), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and Raman scattering, respectively. These results show that the main chemical components of the grown film were single-crystalline 3C-SiC layers. The 3C-SiC film had a very good crystal quality without twins, defects or dislocations, and a very low residual stress.