• Title/Summary/Keyword: TEM Journal

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Synthesis and Characterization of Graphene and Graphene Oxide Based Palladium Nanocomposites and Their Catalytic Applications in Carbon-Carbon Cross-Coupling Reactions

  • Lee, Minjae;Kim, Bo-Hyun;Lee, Yuna;Kim, Beom-Tae;Park, Joon B.
    • Bulletin of the Korean Chemical Society
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    • v.35 no.7
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    • pp.1979-1984
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    • 2014
  • We have developed an efficient method to generate highly active Pd and PdO nanoparticles (NPs) dispersed on graphene and graphene oxide (GO) by an impregnation method combined with thermal treatments in $H_2$ and $O_2$ gas flows, respectively. The Pd NPs supported on graphene (Pd/G) and the PdO NPs supported on GO (PdO/GO) demonstrated excellent carbon-carbon cross-coupling reactions under a solvent-free, environmentally-friendly condition. The morphological and chemical structures of PdO/GO and Pd/G were fully characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). We found that the remarkable reactivity of the Pd/G and PdO/GO catalysts toward the cross-coupling reaction is attributed to the high degree of dispersion of the Pd and PdO NPs while the oxidative states of Pd and the oxygen functionalities of graphene oxide are not critical for their catalytic performance.

SBA-15 Supported Fe, Ni, Fe-Ni Bimetallic Catalysts for Wet Oxidation of Bisphenol-A

  • Mayani, Suranjana V.;Mayani, Vishal J.;Kim, Sang Wook
    • Bulletin of the Korean Chemical Society
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    • v.35 no.12
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    • pp.3535-3541
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    • 2014
  • Bisphenol A is considered as pollutant, because it is toxic and hazardous to living organisms even at very low concentrations. Biological oxidation used for removing this organic from waste water is not suitable and consequently application of catalytic wet oxidation has been considered as one of the best options for treating bisphenol A. We have developed Fe/SBA-15, Ni/SBA-15 and Fe-Ni/SBA-15 as heterogeneous catalysts using the advanced impregnation method for oxidation of bisphenol A in water. The catalysts were characterized with physico-chemical characterization methods such as, powder X-ray diffraction (PXRD), FT-IR measurements, N2 adsorption-desorption isotherm, thermo-gravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis. This work illustrates activity of the catalysts for heterogeneous catalytic degradation reaction revealed with excellent conversion and recyclability. The degradation products identified were not persistent pollutants. GC-MS analysis identified the products: 2,4-hexadienedioic acid, 2,4-pentadienic acid and isopropanol or acetic acid. The leachability study indicated that the catalysts release very little metals to water. Therefore, the possibility of water contamination through metal leaching was almost negligible.

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 $Pr^{3+}$.

Structural Properties of Epoxy-Montmorillonite Nanocomposites (몬모릴로나이트와 에폭시수지로부터 합성된 나노복합재료의 구조적 특성에 관한 연구)

  • Sur, Gil-Soo;Ryu, Joung-Gul;Lyu, Sung-Gyu;Choi, Hyun-Kuk;Kim, Bong-Sik
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.615-619
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    • 1999
  • Polyether-clay nanocomposite was not polymerized with stearyltrimethylammonium ion exchanged montmorillonite, but it was self-polymerizable when heated with both stearyltrimethylammpmoim and m-phenylenediammonium ions intercalated montmorillonite to form polyether-clay nanocomposites. Molcular disperion of montmorillonite within the crosslinked epoxy matrix verified using X-ray diffraction and transmission electron microscopy found that the final product contains a uniform dispersion of exfoliated $10{\AA}$ thin clay layers seperated by $250{\sim}500{\AA}$of polyether polymer, thus verifying the nanocomposite structure.

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A model for Phase Transformation of Microalloyed Low Carbon Steel Combined with Nb Precipitation Kinetics (Nb 석출 거동을 고려한 저탄소강의 상변태 모델)

  • Kim, D.W.;Cho, H.H.;Park, S.;Kim, S.H.;Kim, M.J.;Lee, K.;Han, H.N.
    • Transactions of Materials Processing
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    • v.26 no.1
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    • pp.48-54
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    • 2017
  • The dissolution and precipitation of Nb, which has been known as strong carbide-forming element, play a key role in controlling phase transformation kinetics of microalloyed steels. In this study, we analyzed both numerically and experimentally the precipitation behavior of Nb-microalloyed steel and its effect on the austenite decomposition during cooling. Nb precipitation in austenite matrix could be predicted by the thermo-kinetic software MatCalc, in which interfacial energy between precipitate and matrix is calculated. The simulated precipitation kinetics fairly well agrees with the experimental observations by TEM. Austenite decomposition, which is strongly affected by Nb precipitation during cooling, was measured by dilatometry and was modeled on the basis of a Johnson-Mehl-Avrami-Kolmorgorov(JMAK) equation. It was confirmed that the dissolved Nb delays the austenite decomposition, whereas, the precipitated Nb accelerates phase transformation during the austenite decomposition.

Effect of Support in HI Decomposition Reaction using Pt Catalyst (Pt 촉매를 이용한 HI분해반응에서 지지체에 따른 영향)

  • Ko, Yun-Ki;Park, Chu-Sik;Kang, Kyoung-Soo;Bae, Ki-Kwang;Kim, Young-Ho
    • Journal of Hydrogen and New Energy
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    • v.22 no.4
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    • pp.415-423
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    • 2011
  • HI decomposition step certainly demand catalytic reaction for efficient production of hydrogen in SI process. Platinum catalyst can apply to HI decomposition reaction as well as hydrogenation or dehydrogenation. Generally, noble metal is used as catalyst which is loaded form for getting high dispersion and wide active area. In this study, Pt was loaded onto zirconia, ceria, alumina, and silica by impregnation method. HI decomposition reaction was carried out under the condition of $450^{\circ}C$, 1atm, and $167.76h^{-1}$ (WHSV) in a fixed bed reactor for measuring catalytic activity. And property of a catalyst was observed by BET, TEM, XRD and chemisoption analysis. On the basis of experimental results, we discussed about conversion of HI according to physical properties of the loaded Pt catalyst onto each support.

Novel solvothermal approach to hydrophilic nanoparticles of late transition elements and its evaluation by nanoparticle tracking analysis

  • Dutilleul, Marion Collart;Seisenbaeva, Gulaim A.;Kessler, Vadim G.
    • Advances in nano research
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    • v.2 no.2
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    • pp.77-88
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    • 2014
  • Solvothermal treatment of late transition metal acetylacetonates in a novel medium composed either of pure acetophenone or acetophenone mixtures with amino alcohols offers a general approach to uniform hydrophilic metal nanoparticles with high crystallinity and low degree of aggregation. Both pure metal and mixed-metal particles can be accesses by this approach. The produced materials have been characterized by SEM-EDS, TEM, FTIR in the solid state and by Nanoparticle Tracking Analysis in solutions. The chemical mechanisms of the reactions producing nanoparticles has been followed by NMR. Carrying out the process in pure acetophenone produces palladium metal, copper metal with minor impurity of $Cu_2O$, and NiO. The synthesis starting from the mixtures of Pd and Ni acetylacetonates with up to 20 mol% of Pd, renders in minor yield the palladium-based metal alloy along with nickel oxide as the major phase. Even the synthesis starting from a mixed solution of $Cu(acac)_2$ and $Ni(acac)_2$ produces oxides as major products. The situation is improved when aminoalcohols such as 2-aminoethanol or 2-dimethylamino propanol are added to the synthesis medium. The particles in this case contain metallic elements and pairs of individual metals (not metal alloys) when produced from mixed precursor solutions in this case.

Light and Electron Microscopic Observations on Erythrolobus coxiae gen.et sp.nov. (Porphyridiophyceae, Rhodophyta) from Texas U.S.A.

  • Scott , Joseph L.;Baca, Bart;Ott, Franklyn D.;West, John A.
    • ALGAE
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    • v.21 no.4
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    • pp.407-416
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    • 2006
  • Low molecular weight carbohydrates, phycobilin pigments and cell structure using light and transmission electron microscopy were used to describe a new genus of unicellular red algae, Erythrolobus coxiae (Porphyridiales, Porphyrideophyceae, Rhodophyta). The nucleus of Erythrolobus is located at the cell periphery and the pyrenoid, enclosed by a cytoplasmic starch sheath, is in the cell center. The pyrenoid matrix contains branched tubular thylakoids and four or more chloroplast lobes extend from the pyrenoid along the cell periphery. A peripheral encircling thylakoid is absent. The Golgi apparatus faces outward at the cell periphery and is always associated with a mitochondrion. Porphyridium and Flintiella, the other members of the Porphyrideophyceae, also lack a peripheral encircling thylakoid and have an ER-mitochondria-Golgi association. The low molecular weight carbohydrates digeneaside and floridoside are present, unlike both Porphyridium and Flintiella, which have only floridoside. The phycobilin pigments B-phycoerythrin, R-phycocyanin and allophycocyanin are present, similar to Porphyridium purpureum. The cells have a slow gliding motility without changing shape and do not require substrate contact. The ultrastructural features are unique to members of the Porphyrideophyceae and recent molecular analyses clearly establish the validity of this new red algal class and the genus Erythrolobus.

Degradation of Thermal Creep by Hydrides of Zr-2/5Nb Pressure Tube (Zr-2.5Nb 압력관의 수소화물에 의한 고온 크리프의 열화거동)

  • Oh, Dong-Joon;Ma, Young-Wha;Yoon, Kee-Bong;Kim, Young-Suk
    • Transactions of the Korean Society of Mechanical Engineers A
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    • v.30 no.12 s.255
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    • pp.1526-1533
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    • 2006
  • The aim of this research was to confirm the existence of the thermal creep degradation by hydrides of Zr-2.5Nb pressure tube materials. Small punch creep tests were performed to obtain the relationship between a creep displacement and a loading period at $300^{\circ}C$. A creep stress and a creep strain rate were also converted from the previous results. The creep material constants and the creep stress exponents at the different hydride contents were compared. Finally the hydrides of the axial and circumferential section were observed using OM, SEM and TEM. The following conclusions were made: 1) The degradation of the thermal creep by hydrides was existed and it strongly depended on the hydride contents. 2) As the hydride contents were increased, the creep stress exponents (m) were also increased. 3) Even though the hydride was not precipitated in 50 ppm materials at $300^{\circ}C$, the degradation of thermal creep was found. Therefore, it was believed that this phenomenon strongly related to the hydride precipitation at room temperature.

Effects of Particle Shapes on Unipolar Diffusion Charging of Non-Spherical Particles (비구형 입자의 형상에 따른 단극 확산 하전 특성)

  • Oh, Hyun-Cheol;Park, Hyung-Ho;Kim, Sang-Ho
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.28 no.5
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    • pp.501-509
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    • 2004
  • Unipolar diffusion charging of non-spherical particles was investigated for various particle shapes. We researched with TiO$_2$agglomerates produced by the thermal decomposition of titanium tetraisopropoxide (TTIP) vapor. TTIP was converted into TiO$_2$, in the furnace reactor and was subsequently introduced into the sintering furnace. Increasing the temperature in the sintering furnace, aggregates were restructured into higher fractal dimensions. The aggregates were classified according to their mobility using a differential mobility analyzer. The projection area and the mass fractal dimension of particles were measured with an image processing technique performed by using transmission electron microscope (TEM) photograph. The selected aggregates were charged by the indirect photoelectric-charger and the average number of charges per particle was measured by an aerosol electrometer and a condensation particle counter. For the particles of same mobility diameter, our results showed that the particle charge quantity decreases as the sintering temperature increases. This result is understandable because particles with lower fractal dimension have larger capacitance and geometric surface area.