• Korean Chemical Engineering Research
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• v.51 no.4
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• pp.443-454
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• 2013

Various metal ions (transition and base metals) incorporated MCM-41 catalysts can be synthesized using colloidal and soluble silica with non-sodium involved process. Transition metal ion-typically $V^{5+}$, $Co^{2+}$, and $Ni^{2+}$-incorporated MCM-41 catalysts were synthesized by isomorphous substitution of Si ions in the framework. Each incorporated metal ion created a single species in the silica framework, single-site solid catalyst, showing a substantial stability in reduction and catalytic activity. Radius of pore curvature effect was investigated with Co-MCM-41 by temperature programmed reduction (TPR). The size of metallic Co clusters, sub-nanometer, could be controlled by a proper reduction treatment of Co-MCM-41 having different pore size and the initial pH adjustment of the Co-MCM-41 synthesis solution. These small metallic clusters showed a high stability under a harsh reaction condition without serious migration, resulting from a direct anchoring of small metallic clusters to the partially or unreduced metal ions on the surface. After a complete reduction, partial occlusion of the metallic cluster surface by amorphous silica stabilized the particles against aggregations. As a probe reaction of particle size sensitivity, carbon single wall nanotubes (SWNT) were synthesized using Co-MCM-41. A metallic cluster stability test was performed by CO methanation using Co- and Ni-MCM-41. Methanol and methane partial oxidations were carried out with V-MCM-41, and the radius of pore curvature effect on the catalytic activity was investigated.

• Resources Recycling
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• v.22 no.5
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• pp.13-19
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• 2013

The effect of pH on the citrate leaching behavior of heavy metal ion was investigated to develop an eco-friendly process for removing heavy metals from soil contaminated with copper, zinc, and lead. The leaching tests were performed using citrate solution with pH adjusted by mixing citric acid and sodium citrate under the following leaching conditions: particle size, under $75{\mu}m$; temperature, $50^{\circ}C$; citrate concentration, $1kmol/m^3$; pulp density, 5%; shaking speed, 100 rpm; leaching time, 1 hour. The difference of pH before and after the leaching test was not observed, and this result indicates the direct effect of hydrogen ion concentration on the leaching of metals was insignificant. The removal ratios of copper, zinc, and lead from the contaminated soil decreased with increasing pH. The thermodynamic calculation suggests that the leaching behaviors of metal ions were determined by two reactions; one is the reaction to form complex ions between heavy metal ions and citrate ion species, and the other is the reaction to form metal hydroxide between heavy metal ions and hydroxide ion.

• KSBB Journal
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• v.24 no.4
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• pp.367-376
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• 2009

In this study, two supercritical extraction systems of different scale, analytical-scale and lab-scale, were employed to investigate the extraction efficiency of canola oil from canola seeds using supercritical carbon dioxide ($SCCO_2$) as an extraction solvent. The effects of various parameters such as extraction temperature ($40{\sim}80^{\circ}C$), pressure (200~500 bar), particle size, and $SCCO_2$ flow direction on the extraction rate and yield were examined in detail. Triglycerides and fatty acids in the extracted canola oil were analyzed quantitatively by high-performance liquid chromatography and gas chromatography. The solubility values of canola oil in $SCCO_2$ could be calculated from the experimental results. Similar extraction yields were obtained from both analytical-scale and lab-scale extraction systems. The extraction rates obtained under solvent ($SCCO_2$ ) upflow conditions were found to be higher than those of solvent downflow extraction. However, the effect of $SCCO_2$ flow direction on the extraction yield was observed to be relatively insignificant.

• Transactions of the Korean Society of Mechanical Engineers B
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• v.35 no.10
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• pp.997-1003
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• 2011

In order to investigate devolatilization characteristics for ashless coal with relatively low ash content and high heating value, an experiment was performed in different bed configurations of TGA and DTF(Drop Tube Furnace) at atmospheric pressure condition. The heating rate was $10^{\circ}C$/min up to $950^{\circ}C$ in TGA, while the temperatures of DTF varied from 500 to $1300^{\circ}C$ in step of $200^{\circ}C$. A weight loss and particle temperature were obtained to determine devolatilization kinetics. The kinetic parameters including an activation energy and pre-exponential factor for ashless coal were obtained using Coats-Redfern method in TGA and single step method in DTF. Furthermore, the devolatilization kinetics of the ashless coal were compared with the results of different kinds of conventional coal such as sub-bituminous and bituminous. The results show that the activation energy of devolatilazation for ashless coal is lower than those of others in fixed and entrained conditions.

• Journal of the Korean Magnetics Society
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• v.24 no.2
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• pp.51-55
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• 2014

The $Fe_3O_4$ nanoparticle was synthesized by the hot-injection method while varying the injection time of the precursor solution. The crystal structure was determined to be cubic inverse spinel with space group of Fd-3m based on X-ray diffraction (XRD) measurements and the morphology of the prepared $Fe_3O_4$ nanoparticle was studied with a high-resolution transmission electron microscope (HR-TEM). When the precursor solution was injected for 0.5 min, the size of the $Fe_3O_4$ nanoparticle was 7.63 nm, while the size of the obtained particle was 21.27 nm with the injection time of 60 min. The magnetic properties of the prepared $Fe_3O_4$ nanoparticle were investigated by both vibrating sample magnetometer (VSM) and $^{57}Co$ M$\ddot{o}$ssbauer spectroscopy at various temperatures. From the hyperthermia measurement, we observed that the temperature of the $Fe_3O_4$ nanoparticle powder reached around $120^{\circ}C$ under 250 Oe at 50 kHz, when the injection time of the precursor solution was 60 min.

• Journal of the Korean Magnetics Society
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• v.24 no.3
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• pp.81-85
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• 2014

Nano-sized Ba-ferrite, Ni-Zn ferrite and $BaFe_{12}O_{19}/Ni_{0.5}Zn_{0.5}Fe_2O_4$ nanocomposite ferrite were prepared by sol-gel combustion method. Nanocomposite was calcined at temperature range of $600{\sim}900^{\circ}C$ for 1 h. According to the diffraction patterns, hard/soft nanocomposite was indicated to the coexistence of the magnetoplumbite structural $BaFe_{12}O_{19}$ and spinel $Ni_{0.5}Zn_{0.5}Fe_2O_4$ and agree with the standard data (JCPDS 10-0325). The particle size of nanocomposite turn out to be less than 90 nm. The nanocomposite ferrite shows a single-phase magnetization behavior, implying that the hard magnetic phase and soft magnetic phase were well exchange-coupled. The specific saturation magnetization ($M_s$) of the nanocomposite is located between hard ($BaFe_{12}O_{19}$) and soft ferrite ($Ni_{0.5}Zn_{0.5}Fe_2O_4$). The remanence (Mr) of nanocomposite ferrite is much higher than that for the individual $BaFe_{12}O_{19}$ and $Ni_{0.5}Zn_{0.5}Fe_2O_4$ ferrite. $(BH)_{max}$ is increased, generally.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.26 no.5
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• pp.193-200
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• 2016

Characteristics of $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphorescent phosphors synthesized by solid state reaction and polymerized complex method were comparatively analyzed. In order to evaluate thermal stability of $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphorescent phosphors at high temperature, phosphorescent properties of $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ were investigated with thermal treatment at $1250^{\circ}C$ under reducing atmosphere, which was the general heat treatment conditions for ceramic manufacturing process. The phosphorescent properties of thermally treated $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphors synthesized by solid state reaction and polymerized complex method were investigated. The crystal structure and crystallite size were observed through XRD analysis. Microstructure and particle size of thermally treated $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphors were analyzed by SEM and PSA. Photoluminescence and afterglow characteristics of thermally treated $SrAl_2O_4:Eu^{2+}$, $Dy^{3+}$ phosphorescent phosphors were measured by spectrofluorometer.

• Journal of the Korean Chemical Society
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• v.54 no.2
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• pp.192-197
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• 2010

The spinel compound was obtained by the thermal decomposition of Zn-Co and Zn-Ni gel prepared by sol-gel method using oxalic acid as a chelating agent. The formation of spinel compound has been comfirmed by thermogravimetric analysis (TGA), x-ray powder diffraction (XRD) and infrared spectroscopy (IR). The particle size of 13 nm~16 nm was calculated by Scherrer's equation. The sol-gel method provides a practicable and effective route for the synthesis of the spinel compound at low temperature ($350^{\circ}C$). The kinetic parameters such as activation energy (Ea) and pre-exponential factor (A) for each compound were found by means of the Kissinger method and Arrhenius equation. The decomposition of spinel compound has an activation energy about 155 kJ/mol. Finally, the thermodynamic parameters (${\Delta}G^{\varphi}$, ${\Delta}H^{\varphi}$, ${\Delta}S^{\varphi}$) for decomposition of spinel compound was determined.

• Journal of the Korean Chemical Society
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• v.50 no.2
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• pp.163-177
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• 2006

Alpha Nickel hydroxide samples have been synthesized by electrodeposition on platinum and nickel substrates at current densities of 1, 5, 6, 7 and 10 mAcm？2 at a controlled temperature of 30.00 oC from Ni(NO3)2 bath. Platinum substrate shows a tendency to incorporate less nitrate ions with increase in current density thus producing less hydroxy-deficient nickel hydroxide layers. On the whole the interlayer distance (d003) is found to be inversely proportional to the amount of nitrate ions incorporated in-between the lattice. For the first time we have observed a decrease in lattice spacing with increase in concentration of intercalant (anions) and the reason for lattice contraction is attributed to the columbic attractive forces exerted by the oppositely charged nitrate ion and positively charged slabs. The Infrared spectra of the samples with expanded interlayers show two types of OH vibrations corresponding to hydrogen bonded and non-hydrogen bonded OH groups whereas the contracted interlayers show only hydrogen-boded OH groups. Although the faradaic efficiency is found to increase with increase in applied current there is a local minimum at 6.0 mAcm？2 current density on both platinum and nickel substrates. In this manuscript, GC-MS data is provided which clearly demonstrates the electrodeposited nickel hydroxide sample to consist of huge amount of carbonate ions although the electrolyte solution in nickel nitrate.

• Korean Journal of Optics and Photonics
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• v.16 no.2
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• pp.168-173
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• 2005

Ag-doped $TiO_2$ thin films were prepared by RF magnetron co-sputtering method, and their physical and chemical properties were examined as a function of calcination temperature. XRD results showed that the crystallite size of Ag-doped films was smaller than that of the $TiO_2$ thin films. SEM results showed that the particle size of $Ag/TiO_2$ film was smaller and more uniform than pure $TiO_2$ film. The films had high transparency in the visible range. The films calcined at $600^{\circ}C$ were the anatase phase, and the films calcined at $900^{\circ}C$ were a mixture of anatase and rutile phases. The absorption edge of films calcined at $900^{\circ}C$ was red-shifted. This is due to the augmented absorption resulting from the phase transformation from anatase to rutile phase. And the transmittance of films decreased by the light scattering and absorption in the films. Photocatalytic activity of $Ag/TiO_2$ thin films was higher than that of the pure $TiO_2$ thin films.