• Title/Summary/Keyword: TEM Journal

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Effect of Carbon-coated Silicon/Graphite Composite Anode on the Electrochemical Properties

  • Kim, Hyung-Sun;Chung, Kyung-Yoon;Cho, Byung-Won
    • Bulletin of the Korean Chemical Society
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    • v.29 no.10
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    • pp.1965-1968
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    • 2008
  • The effects of carbon-coated silicon/graphite (Si/Gr.) composite anode on the electrochemical properties were investigated. The nanosized silicon particle shows a good cycling performance with a reasonable value of the first reversible capacity as compared with microsized silicon particle. The carbon-coated silicon/graphite composite powders have been prepared by pyrolysis method under argon/10 wt% propylene gas flow at $700{^{\circ}C}$ for 7 h. Transmission electron microscopy (TEM) analysis indicates that the carbon layer thickness of 5 nm was coated uniformly onto the surface silicon powder. It is confirmed that the insertion of lithium ions change the crystalline silicon phase into the amorphous phase by X-ray diffraction (XRD) analysis. The carbon-coated composite silicon/graphite anode shows excellent cycling performance with a reversible value of 700 mAh/g. The superior electrochemical characteristics are attributed to the enhanced electronic conductivity and low volume change of silicon powder during cycling by carbon coating.

Synthesis of Poly(methacrylic acid)-functionalized SBA-15 and its Adsorption of Phenol in Aqueous Media

  • Vo, Vien;Kim, Hee-Jin;Kim, Ha-Yeong;Kim, Youngmee;Kim, Sung Jin
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3570-3576
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    • 2013
  • Poly(methacrylic acid)-functionalized SBA-15 silicas (denoted as P-x-PMA/SBA-15 where x is molar ratio of TSPM/(TEOS+TSPM) in percentage in the initial mixture) were synthesized by co-condensation of tetraethoxysilane and varying contents of 3-(trimethoxysilyl)propyl methacrylate in acidic medium with the block copolymer Pluronic 123 as a structure directing agent and then polymerization by methacrylic acid in the presence of ammonium persulfate as an initiator. The functionalized materials were characterized by PXRD, TEM, SEM, IR, and $N_2$ adsorption-desorption at 77 K. The investigation of phenol adsorption in aqueous solution on the materials showed that the poly(methacrylic acid)-functionalized mesoporous silicas possess strong adsorption ability for phenol with interaction of various kinds of hydrogen bonds. The adsorption data were fitted to Langmuir isotherms and the maximum adsorption capacity of the three functionalized materials P-5-PMA/SBA-15, P-10-PMA/SBA-15, and P-15-PMA/SBA-15 to be 129.37 mg/g, 187.97 mg/g, and 78.43 mg/g, respectively, were obtained. The effect of the pH on phenol adsorption was studied.

Facile Modification of Surface of Silica Particles with Organosilanepolyol and Their Characterization

  • Lee, Joongseok;Han, Joon Soo;Yoo, Bok Ryul
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3805-3810
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    • 2013
  • The surface modification of silica particles (SPs) was systemically conducted by the treatment of 0.1-10 wt % phenylsilanetriol (PST) on the basis of SPs used through two step processes: 1) the PST coating of SPs via evaporation under reduced pressure and 2) their thermal condensation leading to Si-O-Si bond formation via heating at $130^{\circ}C$. The evaluation of the modified SPs was conducted by the simple floating test on water and the measurement of the contact angle (CA) of water droplet on the 2-dimensional layer of modified SPs on slide glass. When PST was used about 2 wt % or above on the basis of SPs (about average size: 50 nm) used, the modified SPs were fully floated on the water and all dispersed into upper organic solvent layer after a shaking with the mixture of the water and benzene, indicating that the modified SPs have hydrophobic properties. The modified SPs were characterized by $^{29}Si$ MAS NMR and physicochemical properties including SEM, TEM, BET, adsorption/desorption isotherms, etc. were measured and compared each other in details. This research demonstrates that the organosilanetriol is a good modifier applicable for the surface modification of inorganic oxide particles using a low amount of modifier on the basis of oxide particles used.

Transmission Electron Microscopy Characterization of Early Pre-Transition Oxides Formed on ZIRLOTM

  • Bae, Hoyeon;Kim, Taeho;Kim, Ji Hyun;Bahn, Chi Bum
    • Corrosion Science and Technology
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    • v.14 no.6
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    • pp.301-312
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    • 2015
  • Corrosion of zirconium fuel cladding is known to limit the lifetime and reloading cycles of fuel in nuclear reactors. Oxide layers formed on ZIRLO4^{TM}$ cladding samples, after immersion for 300-hour and 50-day in a simulated primary water chemistry condition ($360^{\circ}C$ and 20 MPa), were analyzed by using the scanning transmission electron microscopy (STEM), in-situ transmission electron microscopy (in-situ TEM) with the focused ion beam (FIB) technique, and X-ray diffraction (XRD). Both samples (immersion for 300 hours and 50 days) revealed the presence of the ZrO sub-oxide phase at the metal/oxide interface and columnar grains developed perpendicularly to the metal/oxide interface. Voids and micro-cracks were also detected near the water/oxide interface, while relatively large lateral cracks were found just above the less advanced metal/oxide interface. Equiaxed grains were mainly observed near the water/oxide interface.

Synthesis of Zr-incorporated TiO2 Using a Solvothermal Method and its Photovoltaic Efficiency on Dye-sensitized Solar Cells

  • Kim, Su-Jung;Kang, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • v.32 no.9
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    • pp.3317-3322
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    • 2011
  • This study examines the photoelectric conversion efficiency of dye-sensitized solar cells (DSSCs) when nanometer-sized Zr (0.1, 0.5, and 1.0 mol %)-$TiO_2$ prepared using a solvothermal method is utilized as the working electrode material. The particle sizes observe in the transmission electron microscopy (TEM) images are < 30 nm in all samples. The absorption band is slightly broadened at the tail for the 0.1 mol % Zr-$TiO_2$, and the intensity of the photoluminescence (PL) curves of the Zr-incorporated $TiO_2$ is significantly smaller than that of the pure $TiO_2$. Compared to that using pure $TiO_2$, the energy conversion efficiency is enhanced considerably by the application of Zr-$TiO_2$ in the DSSCs to approximately 6.17% for 0.5 mol % Zr-$TiO_2$ with the N719 dye (10.0 ${\mu}m$ film thickness and 5.0 mm ${\times}$ 5.0 mm cell area) under 100 mW/$cm^2$ of simulated sunlight.

Cytotoxic Potentials of Tellurium Nanowires in BALB/3T3 Fibroblast Cells

  • Mahto, Sanjeev Kumar;Vinod, T.P.;Kim, Jin-Kwon;Rhee, Seog-Woo
    • Bulletin of the Korean Chemical Society
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    • v.32 no.9
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    • pp.3405-3410
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    • 2011
  • We have investigated the cytotoxic potential of tellurium (Te) nanowires in BALB/3T3 fibroblast cells. Te nanowires were synthesized through an aqueous phase surfactant assisted method. Toxicological experiments, such as analysis of morphological changes, MTT assay, DAPI staining, and estimation of intracellular reactive oxygen species, were carried out to reveal the cytotoxic effects of Te nanowires. Te nanowires were found to be cytotoxic at all concentrations tested, in a dose-dependent manner. The UV/Vis spectra of Te nanowires suspended in a culture medium showed drastic changes and disappearance of two broad absorption peaks. The physicochemical properties such as, surface charge, size, and shape of Te nanowires were found to be altered during exposure of cells, due to the instability and agglomeration of nanowires in the culture medium. These results suggest that the chemical components of the DMEM medium significantly affect the stability of Te nanowires. In addition, TEM images revealed that necrosis was the basic pattern of cell death, which might stem from the formation of toxic moieties of tellurium, released from nanowire structures, in the bioenvironment. These observations thus suggest that Te nanomaterials may pose potential risks to environmental and human health.

Suzuki-Miyaura Cross-coupling Reaction Catalyzed by Nickel Nanoparticles Supported on Poly(N-vinyl-2-pyrrolidone)/TiO2-ZrO2 Composite

  • Kalbasi, Roozbeh Javad;Mosaddegh, Neda
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2584-2592
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    • 2011
  • Nickel nanoparticle-poly(N-vinyl-2-pyrrolidone)/$TiO_2-ZrO_2$ composite (Ni-PVP/$TiO_2-ZrO_2$) was prepared by in situ polymerization method. The physical and chemical properties of Ni-PVP/$TiO_2-ZrO_2$ were investigated by XRD, FT-IR, BET, TGA, SEM and TEM techniques. The catalytic performance of this novel heterogeneous catalyst was determined for the Suzuki-Miyaura cross-coupling reaction between aryl halides and phenylboronic acid in the presence of methanol-water mixture as solvent. The effects of reaction temperature, the amount of catalyst, amount of support, solvent, and amount of metal for the synthesis of Ni-PVP/$TiO_2-ZrO_2$, were investigated as well as recyclability of the heterogeneous composite. The catalyst used for this synthetically useful transformation showed considerable level of reusability besides very good activity.

A Surfactant-based Method for Carbon Coating of LiNi0.8Co0.15Al0.05O2 Cathode in Li Ion Batteries

  • Chung, Young-Min;Ryu, Seong-Hyeon;Ju, Jeong-Hun;Bak, Yu-Rim;Hwang, Moon-Jin;Kim, Ki-Won;Cho, Kwon-Koo;Ryu, Kwang-Sun
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2304-2308
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    • 2010
  • A $LiNi_{0.8}Co_{0.15}Al_{0.05}O_2$ (LNCAO/C) active material composite cathode was coated with carbon. The conductive carbon coating was obtained by addition of surfactant during synthesis. The addition of surfactant led to the formation of an amorphous carbon coating layer on the pristine LNCAO surface. The layer of carbon coating was clearly detected by FE-TEM analysis. In electrochemical performance, although the LNCAO/C showed similar capacity at low C-rate conditions, the rate capability was improved by the form of the carbon coating at high current discharge state. After 40 cycles of charge-discharge processes, the capacity retention of LNCAO/C was better than that of LNCAO. The carbon coating is effectively protected the surface structure of the pristine LNCAO during Li insertion-extraction.

Wire-like Bundle Arrays of Copper Hydroxide Prepared by the Electrochemical Anodization of Cu Foil

  • La, Duc-Duong;Park, Sung-Yeol;Choi, Young-Wook;Kim, Yong-Shin
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2283-2288
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    • 2010
  • Nanostructured copper compounds were grown by electrochemical anodization of copper foil in aqueous NaOH under varying conditions including electrolyte concentration, reaction temperature, current density, and reaction time. Their morphology and atomic composition were investigated by using SEM, TEM, XRD, EDS and XPS. At the conditions ([NaOH] = 1 M, $20^{\circ}C$, $2\;mA\;cm^{-2}$), wire-like orthorhombic $Cu(OH)_2$ nanobundles with an average width of 100 - 300 nm and length of $10\;{\mu}m$ were synthesized with the preferential [100] growth direction. Furthermore, when the concentration decreased to 0.5 M NaOH, the 1D nanobundle structure became narrower and longer without any change in compositions or crystalline structure. Side reaction pathways appeared to compete with the 1D nanostructure formation channels: the formation of CuO nanoleaves at $50^{\circ}C$ via the sequential dehydration of $Cu(OH)_2$, CuO/$Cu_2O$ aggregates in 4 M NaOH, and $Cu_2O$ nanoparticles and CuO nanosheets at lower current density.

Effect of Phase Change of $MoO_3$ on $H_2$ Spillover Kinetics over Pt/$MoO_3$ (Pt/$MoO_3$ 촉매에서 $MoO_3$ 상변화가 수소 spillover에 미치는 효과)

  • Kim, Jin-Gul;Kim, Seong-Soo;Yoo, Seung-Joon
    • Journal of Hydrogen and New Energy
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    • v.20 no.4
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    • pp.331-336
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    • 2009
  • 수소가 Pt/$MoO_3$로 흡장되는 현상을 XRD, TEM, CO 화학흡착 분석방법을 사용하여 조사하였다. 소성과정은 Pt/$MoO_3$ 촉매의 Chlorine 함유량을 감소하며 박막을 형성하였다. 소성전과 비교하여 수소 흡장량은 소성 후에 증가하였다. Orthorhombic Pt/$MoO_3$은 Hexagonal Pt/$MoO_3$보다 항상 수소 흡장량이 증가하였다. 상대적으로 Hexagonal Pt/$MoO_3$에서 수소 흡장량이 감소하는 이유는 Hexagonal 결정격자 내에 존재하는 $NH_4^+$ 이온에 기인하는 것으로 판단된다. 결정격자 내부로의 수소 침투시 암모니움 이온이 수소내부 기공에 장애물 역할을 하므로, 수소 흡장량이 감소하는 것으로 판단된다.