• Title/Summary/Keyword: TEM Journal

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Bayberry Tannin as Stabilizer for the Synthesis of Highly Active and Reusable Heterogeneous Pd Catalysts and Their Application in the Catalytic Hydrogenation of Olefins

  • Chen, Chen;Lv, Guang;Huang, Xin;Liao, Xue Pin;Zhang, Wen Hua;Shi, Bi
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.403-408
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    • 2012
  • In this study, the homogenous Pd nanoparticles (Pd NPs) were first prepared with bayberry tannin (BT) as the stabilizers. Subsequently, the obtained bayberry tannin-stabilized Pd nanoparticles (BT-Pd) were immobilized onto ${\gamma}-Al_2O_3$ to prepare heterogeneous ${\gamma}-Al_2O_3$-BT-Pd catalysts. Fourier Transformation Infrared Spectrum (FTIR) and X-ray Photoelectron Spectroscopy (XPS) analyses confirmed that the Pd NPs were well stabilized by the phenolic hydroxyl groups of BT. Transmission Electron Microscopy (TEM) observation indicated that the diameter of the Pd NPs can be effectively controlled in the range of 4.2-16.0 nm by varying the amount of BT. It is found that the ${\gamma}-Al_2O_3$-BT-Pd catalysts exhibit highly activity for various olefin hydrogenations. For example, the initial TOF (turnover frequency) of the ${\gamma}-Al_2O_3$-BT-Pd in the allyl alcohol hydrogenation is as high as $12804 mol{\cdot}mol^{-1}{\cdot}h^{-1}$. Furthermore, the ${\gamma}-Al_2O_3$-BT-Pd can be reused 5 times without significant loss of activity, exhibiting a superior reusability as compared with conventionally prepared ${\gamma}-Al_2O_3$-Pd catalysts.

Preparation and Spectroscopic Characterization of Ilmenite-Type $CoTiO_3$ Nanoparticles

  • Zhou, Guo Wei;Lee, Don-Geun;Kim, Young-Hwan;Kim, Chang-Woo;Kang, Young-Soo
    • Bulletin of the Korean Chemical Society
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    • v.27 no.3
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    • pp.368-372
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    • 2006
  • The cobalt titanate, $CoTiO_3$ nanoparticles have been prepared by calcinations of precursor obtained from a mixture of $TiO_2$ and $Co(OH)_2$ in aqueous cetyltrimethylammonium bromide (CTAB) solution. The nanoparticles were investigated with X-ray powder diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and thermogravimetric/differential thermal analysis (TGA/DTA) to determine the crystallite size and the phase composition. The spectroscopic characterizations of these nanoparticles were also done with UV-Vis spectroscopy and FT-Raman spectroscopy. XRD patterns show that $CoTiO_3$ phase was formed at calcinations temperature above 600 ${^{\circ}C}$. UV-Vis absorption spectra indicate that the $CoTiO_3$ nanoparticles have significant red shift to the visible region (400-700 nm) with $\lambda_{max}$ = 500 nm compared to pure $TiO_2$ powder ($\lambda_{max}$ = 320 nm). The new absorption peaks (absorption at 696, 604, 520, 478,456, 383, 336, 267, 238, 208 $c m ^{-1}$), which were not appeared in FT-Raman spectra of P-25, also confirm the formation of Ti-O-Co bonds at above 600 ${^{\circ}C}$ and just not the mixtures of titanium dioxide with cobalt oxides.

Photovoltaic Efficiencies on Dye-Sensitized Solar Cells Assembled with Graphene-Linked TiO2 Anode Films

  • Kim, A-Young;Kim, Ji-Eun;Kim, Min-Young;Ha, Seung-Won;Tien, Ngyen Thi Thuy;Kang, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3355-3360
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    • 2012
  • To promote the photoelectric conversion efficiency of dye-sensitized solar cells (DSSCs), graphene is introduced as a working electrode with $TiO_2$ in this study, because it has great transparency and very good conductivity. XRD patterns indicate the presence of graphene and $TiO_2$ particles in graphene-linked $TiO_2$ samples. Moreover, TEM pictures also show that the nano-sized $TiO_2$ particles are highly dispersed and well-linked onto the thin layered graphene. On the basis of the UV-visible spectra, the band gaps of $TiO_2$, 1.0 wt % graphene-$TiO_2$, 5.0 wt % graphene-$TiO_2$, and 10.0 wt % graphene-$TiO_2$ are 3.16, 2.94, 2.25, and 2.11 eV, respectively. Compared to pure $TiO_2$, the energy conversion efficiency was enhanced considerably by the application of graphene-linked $TiO_2$ anode films in the DSSCs to approximately 6.05% for 0.1 wt % graphene-$TiO_2$ with N719 dye (10.0 mm film thickness and $5.0mm{\times}5.0mm$ cell area) under $100mW/cm^2$ of simulated sunlight. The quantum efficiency was the highest when 1.0 wt % of graphene was used. In impedance curves, the resistance was smallest for 1.0 wt % graphene-$TiO_2$-DSSC.

TiO2/Carbon Composites Prepared from Rice Husk and the Removal of Bisphenol A in Photocatalytic Liquid System

  • Kim, Ji-Yeon;Kwak, Byeong-Sub;Kang, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • v.31 no.2
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    • pp.344-350
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    • 2010
  • The improved photocatalytic performance of a carbon/$TiO_2$ composite was studied for the Bisphenol A (BPA) decomposition. Titanium tetraisopropoxide (TTIP) and a rice husk from Korea were heterogeneously mixed as the titanium and carbon sources, respectively, for 3 h at room temperature, and then thermally treated at $600^{\circ}C$ for 1 h in $H_2$ gas. The transmission electron microscopy (TEM) images revealed that the bulk carbon partially covered the $TiO_2$ particles, and the amount that was covered increased with the addition of the rice husk. The acquired carbon/$TiO_2$ composite exhibited an anatase structure and a novel peak at $2{\theta}=32^{\circ}$, which was assigned to bulk carbon. The specific surface area was significantly enhanced to 123~164 $m^2/g$ in the carbon/$TiO_2$ composite, compared to $32.43m^2/g$ for the pure $TiO_2$. The X-ray photoelectron spectroscopy (XPS) results showed that the Ti-O bond was weaker in the carbon/$TiO_2$ composite than in the pure $TiO_2$, resulting in an easier electron transition from the Ti valence band to the conduction band. The carbon/$TiO_2$ composite absorbed over the whole UV-visible range, whereas the absorption band in the pure$TiO_2$ was only observed in the UV range. These results agreed well with an electrostatic force microscopy (EFM) study that showed that the electrons were rapidly transferred to the surface of the carbon/$TiO_2$ composite compared to the pure $TiO_2$. The photocatalytic performance of the BPA removal was optimized at a Ti:C ratio of 9.5:0.5, and this photocatalytic composite completely decomposed 10.0 ppm BPA after 210 min, whereas the pure $TiO_2$ achieved no more than 50% decomposition under any conditions.

Comparison of the Kinetic Behaviors of Fe2O3 Spherical Submicron Clusters and Fe2O3 Fine Powder Catalysts for CO Oxidation

  • Yoo, Seung-Gyun;Kim, Jin-Hoon;Kim, Un-Ho;Jung, Jin-Seung;Lee, Sung-Han
    • Bulletin of the Korean Chemical Society
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    • v.35 no.5
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    • pp.1379-1384
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    • 2014
  • ${\alpha}-Fe_2O_3$ spherical particles having an average diameter of ca. 420 nm and ${\alpha}-Fe_2O_3$ fine particles (< 10 ${\mu}m$ particle size) were prepared to examine as catalysts for CO oxidation. Kinetic studies on the catalytic reactions were performed in a flow reactor using an on-line gas chromatography system operated at 1 atm. The apparent activation energies and the partial orders with respect to CO and $O_2$ were determined from the rates of CO disappearance in the reaction stage showing a constant catalytic activity. In the temperature range of $150-275^{\circ}C$, the apparent activation energies were calculated to be 13.7 kcal/mol on the ${\alpha}-Fe_2O_3$ spherical submicron clusters and 15.0 kcal/mol on the ${\alpha}-Fe_2O_3$ fine powder. The Pco and $Po_2$ dependencies of rate were investigated at various partial pressures of CO and $O_2$ at $250^{\circ}C$. Zero-order kinetics were observed for $O_2$ on both the catalysts, but the reaction order for CO was observed as first-order on the ${\alpha}-Fe_2O_3$ fine powder and 0.75-order on the ${\alpha}-Fe_2O_3$ spherical submicron clusters. The catalytic processes including the inhibition process by $CO_2$ on the ${\alpha}-Fe_2O_3$ spherical submicron powder are discussed according to the kinetic results. The catalysts were characterized using XRD (X-ray powder diffraction), FE-SEM (field emission-scanning electron microscopy), HR-TEM (high resolution-transmission electron microscopy), and $N_2$ sorption measurements.

Enhancement of Antibacterial Activity of Short Tryptophan-rich Antimicrobial Peptide Pac-525 by Replacing Trp with His(chx)

  • Ahn, Mija;Rajasekaran, Ganesan;Gunasekaran, P.;Ryu, Eun Kyoung;Lee, Ga-Hyang;Hyun, Jae-Kyung;Cheong, Chaejoon;Kim, Nam-Hyung;Shin, Song Yub;Bang, Jeong-Kyu
    • Bulletin of the Korean Chemical Society
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    • v.35 no.9
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    • pp.2818-2824
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    • 2014
  • Trp residue is considered as one of the important constituents in antimicrobial peptides (AMPs) as it presence secured good activities in many cases. However, it is preferable to be changed because of their sensitivity towards light. We have synthesized the short Trp-rich AMP Pac-525 and its analogues to investigate the possibility of His(chx) as possible replacement analogue for Trp in AMPs. Based on the assay result of the antibacterial activity including anti-MRSA activity, His(chx) is considered as good candidate for the Trp replacement. Through these study, we found that His(chx) had several merits to design therapeutic antimicrobial agents compare to Trp in terms of i) increasing antibacterial activity without hemolytic activity, ii) successful in designing the short peptide (only four residues), iii) having anti-MRSA activity, iv) overcoming the light sensitivity. Furthermore, transmission electron microscopy (TEM) and dye leakage experiments suggested that P11 and P16 containing His(chx) kill bacteria via forming pore/ion channels on bacterial cell membranes.

Chemoenzymatic Synthesis of Dual-responsive Amphiphilic Block Copolymers and Drug Release Studies

  • Chen, Peng;Li, Ya-Peng;Wang, Shu-Wei;Meng, Xin-Lei;Zhu, Ming;Wang, Jing-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1800-1808
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    • 2013
  • Dual-responsive amphiphilic block copolymers were synthesized by combining enzymatic ring-opening polymerization (eROP) of ${\varepsilon}$-caprolactone (CL) and ATRP of N,N-dimethylamino-2-ethyl methacrylate (DMAEMA). The obtained block copolymers were characterized by gel permeation chromatography (GPC), $^1H$ NMR and FTIR-IR. The critical micelle concentration (CMC) of copolymer was determined by fluorescence spectra, it can be found that with hydrophilic block (PDMAEMA) increasing, CMC value of the polymer sample increased accordingly, and the CMC value was 0.012 mg/mL, 0.025 mg/mL and 0.037 mg/mL for $PCL_{50}$-b-$PDMAEMA_{68}$, $PCL_{50}$-b-$PDMAEMA_{89}$, $PCL_{50}$-b-$PDMAEMA_{112}$, $PCL_{50}$-b-$PDMAEMA_{89}$ was chosen as drug carrier to study in vitro release profile of anti-cancer drug (taxol). The temperature and pH dependence of the values of hydrodynamic diameter (Dh) of micelles, and self-assembly of the resulting block copolymers in water were evaluated by dynamic light scattering (DLS). The result showed that with the temperature increasing and pH decreasing, the Dh decreased. Drug-loaded nanoparticles were fabricated using paclitaxel as model. Transmission electron microscopy (TEM) and atomic force microscopy (AFM) had been explored to study the morphology of the hollow micelles and the nanoparticles, revealing well-dispersed spheres with the average diameters both around 80 nm. In vitro release kinetics of paclitaxel from the nanoparticles was also investigated in different conditions (pH and temperature, etc.), revealing that the drug release was triggered by temperature changes upon the lower critical solution temperature (LCST) at pH 7.4, and at $37^{\circ}C$ by an increase of pH.

Effect of Manganese Vanadate Formed on the Surface of Spinel Lithium Manganese Oxide Cathode on High Temperature Cycle Life Performance

  • Kim, Jun-Il;Park, Sun-Min;Roh, Kwang Chul;Lee, Jae-Won
    • Bulletin of the Korean Chemical Society
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    • v.34 no.9
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    • pp.2573-2576
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    • 2013
  • Rate capability and cyclability of $LiMn_2O_4$ should be improved in order to use it as a cathode material of lithium-ion batteries for hybrid-electric-vehicles (HEV). To enhance the rate capability and cyclability of $LiMn_2O_4$, it was coated with $MnV_2O_6$ by a sol-gel method. A $V_2O_5$ sol was prepared by a melt-quenching method and the $LiMn_2O_4$ coated with the sol was heat-treated to obtain the $MnV_2O_6$ coating layer. Crystal structure and morphology of the samples were examined by X-ray diffraction, SEM and TEM. The electrochemical performances, including cyclability at $60^{\circ}C$, and rate capability of the bare and the coated $LiMn_2O_4$ were measured and compared. Overall, $MnV_2O_6$ coating on $LiMn_2O_4$ improves the cyclability at high temperature and rate capability at room temperature at the cost of discharge capacity. The improvement in cyclability at high temperature and the enhanced rate capability is believed to come from the reduced contact between the electrode, and electrolyte and higher electric conductivity of the coating layer. However, a dramatic decrease in discharge capacity would make it impractical to increase the coating amount above 3 wt %.

One-step synthesis of dual-transition metal substitution on ionic liquid based N-doped mesoporous carbon for oxygen reduction reaction

  • Byambasuren, Ulziidelger;Jeon, Yukwon;Altansukh, Dorjgotov;Ji, Yunseong;Shul, Yong-Gun
    • Carbon letters
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    • v.17 no.1
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    • pp.53-64
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    • 2016
  • Nitrogen (N)-doped ordered mesoporous carbons (OMCs) with a dual transition metal system were synthesized as non-Pt catalysts for the ORR. The highly nitrogen doped OMCs were prepared by the precursor of ionic liquid (3-methyl-1-butylpyridine dicyanamide) for N/C species and a mesoporous silica template for the physical structure. Mostly, N-doped carbons are promoted by a single transition metal to improve catalytic activity for ORR in PEMFCs. In this study, our N-doped mesoporous carbons were promoted by the dual transition metals of iron and cobalt (Fe, Co), which were incorporated into the N-doped carbons lattice by subsequently heat treatments. All the prepared carbons were characterized by via transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). To evaluate the activities of synthesized doped carbons, linear sweep was recorded in an acidic solution to compare the ORR catalytic activities values for the use in the PEMFC system. The dual transition metal promotion improved the ORR activity compared with the single transition metal promotion, due to the increase in the quaternary nitrogen species from the structural change by the dual metals. The effect of different ratio of the dual metals into the N doped carbon were examined to evaluate the activities of the oxygen reduction reaction.

Epitaxial Growth of Boron-doped Si Film using a Thin Large-grained Si Seed Layer for Thin-film Si Solar Cells

  • Kang, Seung Mo;Ahn, Kyung Min;Moon, Sun Hong;Ahn, Byung Tae
    • Current Photovoltaic Research
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    • v.2 no.1
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    • pp.1-7
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    • 2014
  • We developed a method of growing thin Si film at $600^{\circ}C$ by hot wire CVD using a very thin large-grained poly-Si seed layer for thin-film Si solar cells. The seed layer was prepared by crystallizing an amorphous Si film by vapor-induced crystallization using $AlCl_3$ vapor. The average grain size of the p-type epitaxial Si layer was about $20{\mu}m$ and crystallographic defects in the epitaxial layer were mainly low-angle grain boundaries and coincident-site lattice boundaries, which are special boundaries with less electrical activity. Moreover, with a decreasing in-situ boron doping time, the mis-orientation angle between grain boundaries and in-grain defects in epitaxial Si decreased. Due to fewer defects, the epitaxial Si film was high quality evidenced from Raman and TEM analysis. The highest mobility of $360cm^2/V{\cdot}s$ was achieved by decreasing the in-situ boron doping time. The performance of our preliminary thin-film solar cells with a single-side HIT structure and $CoSi_2$ back contact was poor. However, the result showed that the epitaxial Si film has considerable potential for improved performance with a reduced boron doping concentration.