• Bulletin of the Korean Chemical Society
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• v.33 no.12
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• pp.3987-3992
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• 2012

Silver nanopowders were prepared from silver 2-ethylhexylcarbamate (Ag-EHCB) complexes by simple thermal reduction at $85^{\circ}C$ without any reducing agent in organic solvent. 2-Ethylhexylammonium 2-ethylhexylcarbamate (EHAEHC) was investigated in terms of their abilities to stabilize the silver nanoparticles (Ag-NPs) and its subsequent effects on the preventing aggregation between Ag-NPs. Conditions (concentration of stabilizer and reaction time) used to reduce Ag-EHCB complex were systematically varied to determine their effects on the sizes of Ag-NPs. The formation of the stabilized Ag-NPs were easily monitored by UV-vis spectroscopy and characterized by TGA, TEM, SEM and XRD. When EHAEHC was used as a stabilizer, Ag-NPs of 10-30 nm in diameter were easily obtained in high yield. Silver patterns were obtained from a silver nano-paste by heat treatment at $200^{\circ}C$ in air and were found to have resistivity values of $2.9{\times}10^{-8}\;{\Omega}{\cdot}m$.

• Bulletin of the Korean Chemical Society
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• v.33 no.6
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• pp.1949-1954
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• 2012

We have developed a novel and eco-friendly synthetic route for the preparation of a two-dimensional layered zinc hydroxide with intercalated nitrate anions. The layered zinc hydroxide nitrate, called 'zinc basic salt', was, in general, successfully synthesized, using an electron beam irradiation technique. The 2-propanol solutions containing hydrated zinc nitrate were directly irradiated with an electron-beam at room temperature, under atmospheric conditions, without stabilizers or base molecules. Under electron beam irradiation, the reactive OH radicals were generated by radiolysis of water molecules in precursor metal salts. After further radiolytic processes, the hydroxyl anions might be formed by the reaction of solvated electrons and the OH radical. Finally, the $Zn_5(OH)_8(NO_3)_2{\cdot}2H_2O$ was precipitated by the reaction of zinc cation and hydroxyl anions. Structure and morphology of obtained compounds were characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and high resolution transmission electron microscopy (HR-TEM). The chemical components of the products were determined by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA). The thermal behavior of products was studied by thermogravimetric (TG) and differential thermal analysis (DTA).

• Bulletin of the Korean Chemical Society
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• v.33 no.12
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• pp.4015-4022
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• 2012

Manganese(III) 5-(4-carboxyphenyl)-10,15,20-triphenyl porphyrin chloride (Mn(TCPP)Cl) was grafted through amide bond on silica zeolite Y (HY), zeolite beta ($H{\beta}$) and hexagonal mesoporous silica (HMS). XRD, ICP-AES, $N_2$ physisorption, SEM, TEM, FTIR and thermal analysis were employed to analyse these novel heterogeneous materials. These silica supported catalysts were shown to be used for epoxidation and good shape selectivity was observed. The effect of support structure on catalytic performance was also discussed. The catalytic activity remained when the catalysts were recycled five times. The energy changes about epoxidation of alkenes by $NaIO_4$ and $H_2O_2$ were also computationally calculated to explain the different catalytic efficiency.

• Bulletin of the Korean Chemical Society
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• v.33 no.6
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• pp.1895-1899
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• 2012

$SiO_2$-coated $TiO_2$ composite materials with enhanced photocatalytic activity under UV light was prepared by a simple catalytic hydrolysis method. XRD, TEM, UV-vis spectroscopy, Photoluminescence, FT-IR and XP spectra were used to characterize the prepared samples. The obvious shell-core structure was shown for obtained $SiO_2$@$TiO_2$ sample. The average thickness of the $SiO_2$ coating layer was 2-3 nm. The interaction between $SiO_2$ and $TiO_2$ restrained the recombination of excited electrons and holes. The photocatalytic activities were tested in the degradation of an aqueous solution of a reactive dyestuff, methylene blue, under UV light. The photocatalytic activity of $SiO_2$@$TiO_2$ was much higher than that of P25 and mechanical mixing sample $SiO_2/TiO_2$. The possible mechanism for the photocatalysis was proposed.

• Bulletin of the Korean Chemical Society
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• v.30 no.1
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• pp.193-196
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• 2009

Mesoporous $TiO_2$ material was synthesized from diblock copolymers with ethylene oxide chains via a sol-gel process in aqueous solution. The properties of these materials were characterized with several analytical techniques including field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), wide angle X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) analysis, and Barrett-Joyner-Halenda (BJH) analysis. The mesoporous $TiO_2$ materials calcined at 400${^{\circ}C}$ were found to have specific surface areas 212 $m^2g^-1$, average pore sizes 6.2 nm, and their average crystal sizes were found to be 8.2 nm. The photocatalytic activity of mesoporous $TiO_2$ was characterized with UV-Vis spectroscopy, and it was found to be 5.8 times higher than that of Degussa P25 $TiO_2$ (P25). For deactivation of Escherichia coli, mesoporous $TiO_2$ also has high photocatalytic inactivity than that of P25. Such a high photocatalytic activity is explained with large surface area and small crystal size with wormhole-like mesoporous structure.

• Bulletin of the Korean Chemical Society
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• v.31 no.12
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• pp.3668-3674
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• 2010

Mesoporous SBA-15 was synthesized using tetraethylorthosilicate (TEOS) as the silica source and Pluronic (P123) as the structure-directing agent. The defective Si-OH groups present in SBA-15 were successively grafted with 3-chloropropyltrimethoxysilane (CPTMS) followed by tris-(2-aminoethyl) amine (TAEA) and/or tetraethylenepentamine (TEPA) for effective immobilization of silver nanoparticles. Grafting of TAEA and/or TEPA amine and immobilization of silver nanoparticles inside the channels of SBA-15 was verified by XRD, TEM, IR and BET techniques. The silver nanoparticles immobilized on TAEA and /or TEPA grafted SBA-15 was subjected for electrocatalytic reduction of hydrogen peroxide ($H_2O_2$). The TEPA stabilized silver nanoparticles show higher efficiency for reduction of $H_2O_2$ than that of TAEA, due to higher number of secondary amine groups present in TEPA. The amperometric analysis indicated that both the Ag/SBA-15/TAEA and Ag/SBA-15/TEPA modified electrodes required lower over-potential and hence possess high sensitivity towards the detection of $H_2O_2$. The reduction peak currents were linearly related to hydrogen peroxide concentration in the range between $3{\times}10^{-4}\;M$ and $2.5{\times}10^{-3}\;M$ with correlation coefficient of 0.997 and detection limit was $3{\times}10^{-4}\;M$.

• Bulletin of the Korean Chemical Society
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• v.30 no.3
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• pp.630-635
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• 2009

For use as a photocatalyst, bismuth tungsten oxide, $Bi_2WO_6$, was successfully synthesized by hydrothermal treatment at pH = 11 and heating at 200 ${^{\circ}C}$ for 24h, and samples were subsequently thermal treated at 400, 600, and 800 ${^{\circ}C}$ to increase crystallinity. TEM results revealed that the initial untreated particles were sheet‐shaped, grain size was below 80 nm, and it increased with treated temperatures. These $Bi_2WO_6$ samples absorbed at around 400 nm in the visible light range and the intensity of absorption was particularly strongest in samples thermal treated at 600 ${^{\circ}C}$. Their photoluminescence abilities, related to the recombination between the excited electrons and holes, were overall small for other general photocatalysts such as TiO2, and the smallest in the case of thermal treatment at 600 ${^{\circ}C}$, as reversible result of UV‐visible absorbance. Methyl orange of 5.0 ppm aqueous solution was almost completely removed after 2 h when treated over the $Bi_2WO_6$ thermal treated at 600 ${^{\circ}C}$.

• Bulletin of the Korean Chemical Society
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• v.30 no.11
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• pp.2584-2588
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• 2009

The effect of $LaF_3$ coating on the structural and electrochemical properties of $Li[Ni_{0.3}Co_{0.4}Mn_{0.3}]O_{2}$ cathodes was investigated using XRD, SEM, TEM, and a cycler. The coating layer consisted of nano-sized particles attached nonuniformly to the surface of pristine powder. Despite the surface coating treatment, phase difference by $LaF_3$ coating was not detected. The discharge capacities of coated electrodes were a little lower than that of pristine sample at a 1 C rate. However, as the C rate increases, the capacity retention of the coated sample becomes obviously superior to that of the pristine sample. The cyclic performances of the electrodes in the voltage range of 4.8 $\sim$ 3.0 V were also improved by the surface coating. Such enhancement is attributed to the presence of the $LaF_3$ coating layer, which effectively suppressd the reaction between electrodes and electrolytes on the surface of the $Li[Ni_{0.3}Co_{0.4}Mn_{0.3}]O_{2}$ electrode.

• Bulletin of the Korean Chemical Society
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• v.34 no.1
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• pp.143-148
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• 2013

Novel titanium containing solid core mesoporous shell silica has been synthesized by using octadecyltrichloro silane and triethylamine. The synthesized material was characterized by various physicochemical techniques. The mesoporous character of the material has been revealed from PXRD studies. The presence of octadecyltrichloro silane and triethylamine in the sample has been confirmed from EDAX studies. TG/DTA analysis reveals the thermal characteristics of the synthesized material. The presence of titanium in the frame work and its coordination state has been studies by UV-vis DR studies and XPS analysis. Chemical environment of Si in the framework of the material has been studied by $^{29}SiMASNMR$ studies. The surface area of the material is found to be around $550\;m^2g^{-1}$ and pore radius is of nano range from BET analysis. The spherical morphology and particle size of the core as well as shell has been found to be 300 nm and 50 nm respectively from TEM analysis. The catalytic application of this material towards the synthesis of caprolactam from cyclohexanone in presence of hydrogen peroxide through ammoxidation reaction has been investigated. The optimum conditions for the reaction have been established. The plausible mechanism for the formation of core silica and conversion of cyclohexanone has been proposed.

• Bulletin of the Korean Chemical Society
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• v.34 no.5
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• pp.1333-1338
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• 2013

Chitosan-based nanoparticles (CSNP) were prepared through ionic cross-linking and gelation of chitosan (CS) by tripolyphosphate (TPP). CS properties such as molecular weight, and preparation conditions were screened and the resulting nanoparticles were examined by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The obtained particles were consistently spherical with an overall diameter of approximately $107{\pm}20$ nm. They were successfully used as a carrier for Zidovudine, an anti-human immunodeficiency virus (HIV) which, to our knowledge, is novel. The encapsulation ability, loading capacity, and controlled release behavior for these CSNP was evaluated. Results indicated that their intrinsic properties were strongly affected by properties inherent to CS such as molecular weight, and by the preparation condition, such as cross-linking density, which depends on the concentration of the cross-linker. In vitro release tests for the entrapped zidovudine showed that the CNNP provided a continuous release that can last upwards 20 h.