• Title/Summary/Keyword: TEM Journal

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Catalytic Properties of Ti-HMS with High Titanium Loadings

  • Jang, S.H.;Kim, M.J.;Ko, J.R.;Ahn, W.S.
    • Bulletin of the Korean Chemical Society
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    • v.26 no.8
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    • pp.1214-1218
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    • 2005
  • Ti-HMS samples in which titanium species exist in various forms of isolated tetrahedral state, finely dispersed $TiO_2$ cluster, and some in extra-framework anatase phase were prepared via a direct synthesis route using dodecylamine (DDS) as a structure directing agent by systematically varying the titanium loadings between 2 and 50 mol% Ti/(Ti+Si) in substrate composition. Physicochemical properties of the materials were evaluated using XRD, SEM/TEM, N2 adsorption, UV-vis and XANES spectroscopies. Catalytic properties of Ti-HMS in cyclohexene and 2,6-di-tert-butyl phenol (2,6-DTBP) oxidation using aqueous $H_2O_2$, and vapor phase photocatalytic degradation of acetaldehyde were evaluated. High $H_2O_2$ selectivity was obtained in cyclohexene oxidation, and cyclohexene conversion was found primarily dependent on the amount of tetrahedrally coordinated Ti sites. For bulky 2,6-DTBP oxidation and photocatalytic oxidation of acetaldehyde, on the other hand, conversions were found dependent on the total amount of Ti sites and maintaining an uniform mesoporous structure in the catalysts was not critical for efficient catalysis.

γ-ray Radiation Induced Synthesis and Characterization of α-Cobalt Hydroxide Nanoparticles

  • Kim, Sang-Wook;Kwon, Bob-Jin;Park, Jeong-Hoon;Hur, Min-Goo;Yang, Seung-Dae;Jung, Hyun
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.910-914
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    • 2010
  • A novel synthetic route has been developed to prepare $\alpha$-cobalt hydroxide with intercalated nitrate anions. It was successfully synthesized by $\gamma$-ray irradiation under simple conditions, i.e., air atmosphere, without base. Under $\gamma$-ray irradiation, it leads to the formation of layered cobalt hydroxynitrate compounds which have small crystalline size and have the role of a generator of hydroxyl anion. Structural and morphological characterizations were performed by using power X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and high resolution transmission electron microscopy (HR-TEM). The component and thermal stability of the sample were respectively measured by Fourier transform infrared (FT-IR) spectroscopy, elemental analysis, and thermal analyses, including thermogravimetry (TG) and differential thermal analysis (DTA).

Electrochemical Characteristics of Carbon-coated Si/Cu/graphite Composite Anode

  • Kim, Hyung-Sun;Chung, Kyung-Yoon;Cho, Won-Il;Cho, Byung-Won
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1607-1610
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    • 2009
  • The carbon-coated Si/Cu powder has been prepared by mechanical ball milling and hydrocarbon gas decomposition methods. The phase of Si/Cu powder was analyzed using X-ray diffraction (XRD), dispersive Raman spectroscopy, electron probe microanalysis (EPMA) and transmission electron microscope (TEM). The carbon-coated Si/Cu powders were used as anode active material for lithium-ion batteries. Their electrochemical properties were investigated by charge/discharge test using commercial LiCo$O_2$ cathode and lithium foil electrode, respectively. The surface phase of Si/Cu powders consisted of carbon phase like the carbon nanotubes (CNTs) with a spacing layer of 0.35 nm. The carbon-coated Si/Cu/graphite composite anode exhibited a higher capacity than commercial graphite anode. However, the cyclic efficiency and the capacity retention of the composite anode were lower compared with graphite anode as cycling proceeds. This effect may be attributed to some mass limitations in LiCo$O_2$ cathode materials during the cycling.

Synthesis and Catalytic Applications of Ruthenium(0) Nanoparticles in Click Chemistry

  • Kumar, Avvaru Praveen;Baek, Min-Wook;Sridhar, Chirumarry;Kumar, Begari Prem;Lee, Yong-Ill
    • Bulletin of the Korean Chemical Society
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    • v.35 no.4
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    • pp.1144-1148
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    • 2014
  • Here we report a facile synthesis of ruthenium (Ru) Nanoparticles (NPs) by chemical co-precipitation method. The calcination of ruthenium hydroxide samples at $500^{\circ}C$ under hydrogen atmosphere lead to the formation of $Ru^0$ NPs. The size and aggregation of Ru NPs depends on the pH of the medium, and type of surfactant and its concentration. The X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope image (TEM) analyses of particles indicated the formation of $Ru^0$ NPs, and have 10 to 20 nm sizes. As-synthesized $Ru^0$ NPs are characterized and investigated their catalytic ability in click chemistry (azidealkyne cycloaddition reactions), showing good results in terms of reactivity. Interestingly, small structural differences in triazines influence the catalytic activity of $Ru^0$ nanocatalysts. Click chemistry has recently emerged to become one of the most powerful tools in drug discovery, chemical biology, proteomics, medical sciences and nanotechnology/nanomedicine. In addition, preliminary tests of recycling showed good results with neither loss of activity or significant precipitation.

Synthesis and Optical Characteristics of PAM/HgS Nanocomposites

  • Qin, Dezhi;Yang, Guangrui;Zhang, Li;Du, Xian;Wang, Yabo
    • Bulletin of the Korean Chemical Society
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    • v.35 no.4
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    • pp.1077-1081
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    • 2014
  • Polyacrylamide (PAM) -HgS nanocomposites were successfully prepared in polyacrylamide (PAM) matrix. From TEM and XRD characterizations, the synthesized HgS nanocrystals were chain-like spherical in shape with a diameter of about 40-60 nm and high crystalline quality. The quantum-confined effect of HgS nanocrystals was confirmed by UV-vis diffuse reflection spectra. The optical properties of products were investigated by using photoluminescence (PL) spectra, which showed that HgS nanocrystals exhibited good optical properties with maximum emission peak at about 640 and 650 nm at different reaction temperatures. The interaction of HgS nanocrystals with PAM was studied through FT-IR spectroscopy and TG analysis, which suggested that $Hg^{2+}$ could interact with functional groups of PAM. The experimental results indicated that PAM not only induced nucleation, but also inhibited further growth of HgS crystals and play an important role in the formation of PAM/HgS nanocomposites. In addition, the possible mechanism of HgS nanoparticles growth in PAM solution was also discussed.

Electrochemical Properties of LiNi0.8Co0.16Al0.04O2 and Surface Modification with Co3(PO4)2 as Cathode Materials for Lithium Battery

  • Ryu, Kwang-Sun;Lee, Sang-Hyo;Park, Yong-Joon
    • Bulletin of the Korean Chemical Society
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    • v.29 no.9
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    • pp.1737-1741
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    • 2008
  • The electrochemical and thermal stability of $LiNi_{0.8}Co_{0.16}Al_{0.04}O_2$ were studied before and after $Co_3(PO_4)_2$ coating. Different to conventional coating material such as $ZrO_2$ or AlPO4, the coating layer was not detected clearly by TEM analysis, indicating that the $Co_3(PO_4)_2$ nanoparticles effectively reacted with surface impurities such as $Li_2CO_3$. The coated sample showed similar capacity at a low C rate condition. However, the rate capability was significantly improved by the coating effect. It is associated with a decrease of impedance after coating because impedance can act as a major barrier for overall cell performances in high C rate cycling. In the DSC profile of the charged sample, exothermic peaks were shifted to high temperatures and heat generation was reduced after coating, indicating the thermal reaction between electrode and electrolyte was sucessfully suppressed by $Co_3(PO_4)_2$ nanoparticle coating.

Size control of Co-doped ZnO rods by changing the solvent

  • Zhao, Jing;Yan, Xiaoqin;Lei, Yang;Zhao, Yanguang;Huang, Yunhua;Zhang, Yue
    • Advances in materials Research
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    • v.1 no.1
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    • pp.75-81
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    • 2012
  • In this work, the Co-doped ZnO rods were prepared by the hydrothermal method. The size of these rods can be changed from micro-size to nano-size by using different solutions during the preparation. The results of transmission electron microscopy (TEM) and selected area electron diffraction (SAED) showed that the as-prepared nano-sized Co-doped rods have single-crystal structure. The polarized Raman experiments were presented on an individual micro-sized Co-doped ZnO rod in the $X(YY)\vec{X}$, $X(ZY)\vec{X}$ and $X(ZZ)\vec{X}$ configurations, the results of polarized Raman indicated that these rods are crystallized and their growth direction is parallel to c-axis.

Tunneling the size of iron oxide NPs using different alcohols and proportions water-alcohol

  • Rivera, F.L.;Sanchez-Marcos, J.;Menendez, N.;Herrasti, P.;Mazario, E.
    • Advances in nano research
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    • v.8 no.2
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    • pp.95-102
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    • 2020
  • In this work the properties of iron oxide magnetic nanoparticles (MNPs) synthesized by electrochemical method using different water-alcohol proportions and alcohols have been investigated. The syntheses were carried out using 99% iron foils acting electrodes in a 0.04 M NaCl solutions at room temperature applying 22 mAcm-2 on the working electrode, mostly obtaining magnetite nanoparticles. The impact of the electrolyte in the size of the synthesized MNPs has been evaluated by transmission electron microscopy (TEM), X-ray diffraction (XRD), chronopotentiometric studies, and magnetic characterization. The results have shown that nanoparticles can be obtained in the range of 6 to 26 nm depending on the type of alcohol and the proportions in the mixture of water-alcohol. The same trend has been observed for all alcohols. As the proportion of these in the medium increases, the nanoparticles obtained are smaller in size. This trend is maintained until a certain proportion of alcohol: 50% for methanol, and 60% for the rest of alcohols, proportions where obtaining a single phase of magnetite is not favored.

The Synthesis of Cellulose-graft-poly (L-lactide) by Ring-opening Polymerization and the Study of Its Degradability

  • Dai, Lin;Xiao, Shu;Shen, Yue;Qinshu, Baichuan;He, Jing
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.4122-4126
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    • 2012
  • Cellulose-graft-poly (L-lactide) (cellulose-g-PLLA) was successfully prepared via ring-opening polymerization (ROP) by using 4-dimethylaminopyridine (DMAP) as an organic catalyst in an ionic liquid 1-allyl-3-methylimidazolium chloride (AmimCl). The structure and morphology of the polymer was characterized by nuclear magnetic resonance (NMR) and transmission electron microscope (TEM). From wide-angle X-ray powder diffraction (WAXD) and degradation test (by acid, alkaline, PBS and enzyme solution), changes in the crystalline structure as a result of degradation was also investigated. The results indicated that materials which have low degree of crystallinity showing higher degradability, however, in acid liquor, enzyme solution, alkaline liquor and PBS system, the degradation rate of the polymer decreased by the above sequence. Moreover, with the further increase of graft degree of this material, its degradation degree decreased.

Effect of Oxygen Vacancies on Photocatalytic Efficiency of TiO2 Nanotubes Aggregation

  • Liu, Feila;Lu, Lu;Xiao, Peng;He, Huichao;Qiao, Lei;Zhang, Yunhuai
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2255-2259
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    • 2012
  • Aggregation of titania nanotubes (TNTs) fabricated by hydrothermal method were calcined in air and dry nitrogen; Changes in morphology and crystallinity of the nanotubes were studied by means of TEM, EDX, and XPS. EDX patterns and XPS spectra proved that there were a certain densities of oxygen vacancies in TNTs annealed in $N_2$. The photocatalysis experiments revealed TNTs/$N_2$ possesses significantly higher photocatalytic efficiency than TNTs annealed in dry air to degrade methylene blue. The correlation between oxygen vacancies and photocatalytic property may be attributed to: 1) oxygen vacancies might have affected results on water molecules adsorption and increase of the hydroxyl concentration; and 2) oxygen vacancies resulted in some changes in electronic structure of TNTs/$N_2$ aggregation and Fermi level extends into the conducting band.