• Title/Summary/Keyword: TEM Journal

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Biguanide-Functionalized Fe3O4/SiO2 Magnetic Nanoparticles: An Efficient Heterogeneous Organosuperbase Catalyst for Various Organic Transformations in Aqueous Media

  • Alizadeh, Abdolhamid;Khodaei, Mohammad M.;Beygzadeh, Mojtaba;Kordestani, Davood;Feyzi, Mostafa
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2546-2552
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    • 2012
  • A novel biguanide-functionalized $Fe_3O_4/SiO_2$ magnetite nanoparticle with a core-shell structure was developed for utilization as a heterogeneous organosuperbase in chemical transformations. The structural, surface, and magnetic characteristics of the nanosized catalyst were investigated by various techniques such as transmission electron microscopy (TEM), powder X-ray diffraction (XRD), vibrating sample magnetometry (VSM), elemental analyzer (EA), thermogravimetric analysis (TGA), $N_2$ adsorption-desorption (BET and BJH) and FT-IR. The biguanide-functionalized $Fe_3O_4/SiO_2$ nanoparticles showed a superpara-magnetic property with a saturation magnetization value of 46.7 emu/g, indicating great potential for application in magnetically separation technologies. In application point of view, the prepared catalyst was found to act as an efficient recoverable nanocatalyst in nitroaldol and domino Knoevenagel condensation/Michael addition/cyclization reactions in aqueous media under mild condition. Additionally, the catalyst was reused six times without significant degradation in catalytic activity and performance.

Mesoporous Carbon as a Metal-Free Catalyst for the Reduction of Nitroaromatics with Hydrazine Hydrate

  • Wang, Hui-Chun;Li, Bao-Lin;Zheng, Yan-Jun;Wang, Wen-Ying
    • Bulletin of the Korean Chemical Society
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    • v.33 no.9
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    • pp.2961-2965
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    • 2012
  • Mesoporous carbons with tailored pore size were prepared by using sucrose as the carbon source and silicas as the templates. The silica templates were obtained from a hydroxypropyl-${\beta}$-cyclodextrin-silica hybrids using ammonium perchlorate oxidation at different temperatures to remove the organic matter. The structures and surface chemistry properties of these carbon materials were characterized by $N_2$ adsorption, TEM, SEM and FTIR measurements. The catalytic performances of these carbon materials were investigated through the reduction of nitroaromatic using hydrazine hydrate as the reducing agent. Compared with other carbon materials, such as active carbon, and carbon materials from the silica templates obtained by using calcination to remove the organic matter, these carbon materials exhibited much higher catalytic activity, no obvious deactivation was observed after recycling the catalyst four times. Higher surface area and pore volume, and the presence of abundant surface oxygen-containing functional groups, which originate from the special preparation process of carbon material, are likely responsible for the high catalytic property of these mesoporous carbon materials.

Performance Enhancement by Adaptation of Long Term Chronoamperometry in Direct Formic Acid Fuel Cell using Palladium Anode Catalyst

  • Kwon, Yong-Chai;Baik, S.M.;Han, Jong-Hee;Kim, Jin-Soo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2539-2545
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    • 2012
  • In the present study, we suggest a new way to reactivate performance of direct formic acid fuel cell (DFAFC) and explain its mechanism by employing electrochemical analyses like chronoamperometry (CA) and cyclic voltammogram (CV). For the evaluation of DFAFC performance, palladium (Pd) and platinum (Pt) are used as anode and cathode catalysts, respectively, and are applied to a Nafion membrane by catalyst-coated membrane spraying. After long DFAFC operation performed at 0.2 and 0.4 V and then CV test, DFAFC performance is better than its initial performance. It is attributed to dissolution of anode Pd into $Pd^{2+}$. By characterizations like TEM, Z-potential, CV and electrochemical impedance spectroscopy, it is evaluated that such dissolved $Pd^{2+}$ ions lead to (1) increase in the electrochemically active surface by reduction in Pd particle size and its improved redistribution and (2) increment in the total oxidation charge by fast reaction rate of the Pd dissolution reaction.

Cadmium Sulphide Nanorods: Synthesis, Characterization and their Photocatalytic Activity

  • Giribabu, Krishnamoorthy;Suresh, Ranganathan;Manigandan, Ramadoss;Vijayaraj, Arunachalam;Prabu, Raju;Narayanan, Vengidusamy
    • Bulletin of the Korean Chemical Society
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    • v.33 no.9
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    • pp.2910-2916
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    • 2012
  • Cadmium sulphide (CdS) nanorods were prepared by a single precursor thermal decomposition (SPTD) method. The formation of CdS nanorods and their structure, morphology and elemental composition were studied by means of FT-IR, XRD, FE-SEM, HR-TEM and EDAX analysis. Photoluminescence (PL) and lifetime measurements were recorded to study the luminescence properties of the material. The PL spectrum of the CdS nanorods showed one broad peak and four shoulders and the cause for this emission was discussed. The PL emissions from the band edge and deep trap state of the CdS nanorods were studied by lifetime measurements. Further, the synthesized CdS nanorods showed an increase in efficiency of photocatalytic degradation of methylene blue (MB) and rhodamine B (RhB). The increase in the photocatalytic activity was attributed to the mixed phase of the CdS nanorods.

Characterization and Photonic Effect of Novel Ag-CNT/TiO2 Composites and their Bactericidal Activities

  • Zhang, Feng-Jun;Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1981-1987
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    • 2010
  • A novel composite (Ag-CNT/$TiO_2$) of silver treated carbon nanotubes (Ag-CNT) and $TiO_2$ was synthesized via wet chemistry followed by a heat treatment. The dispersion and structure of the silver in the synthesized composites determined by X-ray diffraction (XRD), energy dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy(TEM). XRD patterns of the composites showed that the composites contained a mixing anatase and rutile phase. The EDX spectra showed the presence of C, O, Ti and Ag peaks. The $TiO_2$ particles were distributed uniformly in the CNT network, and silver particles were virtually fixed on the surface of the tube. The photocatalysis degraded behaviors of the Ag-CNT/$TiO_2$ composites of the methylene blue, which increased with an increase of the silver component. The Ag-CNT/$TiO_2$ composites have excellent antibacterial activities against Escherichia coli (E. Coli), Pseudomonas aeruginosa (P. Aeru) and Bacillus subtilis (B. Sub) under visible light.

A Comparison Method of Silver Nanoparticles Prepared by the Gamma Irradiation and in situ Reduction Methods

  • Lee, Chul-Jae;Karim, Mohammad Rezaul;Vasudevan, T.;Kim, Hee-Jin;Raushan, K.;Jung, Maeng-Joon;Kim, Dong-Yeub;Lee, Mu-Sang
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1993-1996
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    • 2010
  • Silver nanoparticles has been prepared by the $\gamma$-irradiation and in situ reduction methods. Based on the Raman spectra, TEM images, X-ray Diffraction (XRD) patterns and UV-vis spectra, the in situ reduction method is more stable and the average size of the silver nanoparticles is also smaller than by the $\gamma$-irradiation reduction method. It is identified that the silver ions interacting with nonbonding electrons of oxygen atom in the carbonyl group of polyvinylpyrrolidone (PVP) by the in situ reduction method. It is also found advantages of the in situ reduction method including no additional reducing agents, without $\gamma$-irradiations treatment and the room temperature treatment suitability.

Protein-Directed Synthesis of γ-Fe2O3 Nanoparticles and Their Magnetic Properties Investigation

  • Soleyman, Rouhollah;Pourjavadi, Ali;Masoud, Nazila;Varamesh, Akbar;Sattari, Abolfazl
    • Bulletin of the Korean Chemical Society
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    • v.35 no.5
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    • pp.1375-1378
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    • 2014
  • In this study, maghemite (${\gamma}-Fe_2O_3$) nanoparticles were produced using gelatin protein as an effective mediator. Size, shape, surface morphology and magnetic properties of the prepared ${\gamma}-Fe_2O_3$ nanoparticles were characterized using XRD, FT-IR, TEM, SEM and VSM data. The effects of furnace temperature and time of heating together with the amount of gelatin on the produced gelatin-$Fe_3O_4$ nanocomposite were examined to prove the fundamental effect of gelatin; both as a capping agent in the nanoscale synthesis and as the director of the spinel ${\gamma}-Fe_2O_3$ synthesis among possible $Fe_2O_3$ crystalline structures.

Ultrafine Copper Nanoparticles Exhibiting a Powerful Antifungal/Killing Activity Against Corticium Salmonicolor

  • Cao, Van Du;Nguyen, Phuong Phong;Khuong, Vo Quoc;Nguyen, Cuu Khoa;Nguyen, Xuan Chuong;Dang, Cap Ha;Tran, Ngoc Quyen
    • Bulletin of the Korean Chemical Society
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    • v.35 no.9
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    • pp.2645-2648
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    • 2014
  • In this paper ultrafine copper nanoparticles (CuNPs) were prepared from copper salt via chemical reduction method with sodium citrate dispersant and polyvinylalcol (PVA) capping polymer. The colloidal CuNPs were characterized by using UV-Visible spectroscopy, Transmission Electron Microscopy (TEM), and X-ray Diffraction (XRD) techniques. Our obtained results indicated that the CuNPs were produced ranging from 2 to 4 nm in diameter. The colloidal solution at 7 ppm of CuNPs exhibited a powerful antifungal activity against Corticium salmonicolor (C. Salmonicolor). Fungal killing assays showed colloid solutions containing 10 ppm of CuNPs killed entirely the cultured fungus. A highly killing activity against the fungus was also performed when the CuNPs were sprayed on pink disease-infected rubber trees. These positive results may offer a great potential to produce CuNPs-based eco-fungicide for pink disease.

Synthesis of Thermally Stable Mesoporous Alumina by using Bayberry Tannin as Template in Aqueous System

  • Liu, Jing;Huang, Fuming;Liao, Xuepin;Shi, Bi
    • Bulletin of the Korean Chemical Society
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    • v.34 no.9
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    • pp.2650-2656
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    • 2013
  • Mesoporous alumina was synthesized using bayberry tannin (BT) as template. This novel synthesis strategy was based on a precipitation method associated with aluminum nitrate as the source of aluminum in an aqueous system. $N_2$ adsorption/desorption, XRD, SEM and TEM were used to characterize the as-prepared mesoporous alumina. The results showed that the mesoporous alumina possessed crystalline pore wall, high specific surface area, narrow pore distribution and excellent thermal stability. Moreover, the surface area and pore size of the mesoporous alumina can be tuned by changing the experimental parameters. Further, the mesoporous alumina was investigated as the support of palladium catalyst ($Pd-Al_2O_3{^*}$) for the hydrogenation of propenyl, styrene and linoleic acid. For comparison, the reference catalyst ($Pd-Al_2O_3$) prepared without barberry tannin was also employed for the catalytic hydrogenation. The experimental results showed that $Pd-Al_2O_3{^*}$ exhibited the superior catalytic performance than $Pd-Al_2O_3$ for all the investigated substrates, especially for the hydrogenation of linoleic acid with larger molecular.

Effects of Hydrogen on the PWSCC Initiation Behaviours of Alloy 182 Weld in PWR Environments

  • Kim, H.-S.;Hong, J.-D.;Lee, J.;Gokul, O.S.;Jang, C.
    • Corrosion Science and Technology
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    • v.14 no.3
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    • pp.113-119
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    • 2015
  • Alloy 82/182 weld metals had been extensively used in joining the components of the PWR primary system. Unfortunately, there have been a number of incidents of cracking caused by PWSCC in Alloy 82/182 welds during the operation of PWR worldwide. To mitigate PWSCC, optimization of water-chemistry conditions, especially dissolved hydrogen (DH) and Zn contents, is considered as the most promising and effective remedial method. In this study, the PWSCC behaviours of Alloy 182 weld were investigated in simulated PWR environments with various DH content. Both in-situ and ex-situ oxide characterizations as well as PWSCC initiation tests were performed. The results showed that PWSCC crack initiation time was shortest in PWR water (DH: 30cc/kg). Also, high stress reduced crack initiation time. Oxide layer showed multi-layered structures consisted of the outer needle-like Ni-rich oxide layer, Fe-rich crystalline oxide, and inner Cr-rich inner oxide layers, which was not altered by the level of applied stress. To analyse the multi-layer structure of oxides, EIS measurement were fitted into an equivalent circuit model. Further analyses including TEM and EDS are underway to verify appropriateness of the equivalent circuit model.