• Bulletin of the Korean Chemical Society
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• 제20권6호
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• pp.715-719
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• 1999

The incorporation of cobalt into mesoporous molecular sieves MCM-41 and MCM-48 was carried out. Co-PO/MCM41 and Co-PO/MCM48 were prepared using Co(II) acetate solution adjusted to pH = 3.0 with phosphoric acid by the incipient wetness method. Photoacoustic spectroscopy (PAS) was used to study the local environments of Co(II) incorporated into mesopores. The band around 500 nm in PAS of as-prepared Co-PO/MCM41 and Co-PO/MCM48 with Co(II) acetate solution was changed to triplet bands around 600 nm. This could be assigned to the 4 A2(F)-> 4T1(P) transition of Co(II) surrounded tetrahedrally by oxygen ions after calcination. It may be attributable to that the octahedral cobalt species containing phosphate ligands in coordination sphere reacting with framework's silanol groups to be dispersed atomically onto the surface of mesoporous molecular sieves as a tetrahedral species. This is unlike that the Co in Co-Cl/MCM41 and direct-synthesized Co-MCM41 transforms to Co oxide phase upon calcination. Co-PO/MCM41 and Co-PO/MCM48 were stable while treated with water.

• 한국결정성장학회지
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• 제16권6호
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• pp.256-259
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• 2006

Vapor phase epitaxy(VPE)법을 사용하여 amorphous $SiO_x$. nanowires를 성장시켰다. Ni thin film을 촉매로 사용하여 Si 기판위에 $800{\sim}1100^{\circ}C$ 범위의 온도에서 성장시켰으며, $SiO_x$ nanowires의 성장 메커니즘은 Vapor-liquid-solid(VLS)으로 확인되었다. $SiO_x$ nanowires의 shape와 morphology는 scanning electron microscope(SEM)으로 분석하였으며, cotton-like형태이고 길이는 $10{\mu}m$정도였다. 그리고 구조적 특징은 transmission electron microscope(TEM)으로 관찰하였고, $SiO_x$ nanowires의 성분 분석은 energy dispersed X-ray spectroscopy(EDS)로 하였다. EDX spectrum으로 nanowires가 Si와 O로 구성되어졌음을 확인하였다.

• Bulletin of the Korean Chemical Society
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• 제34권10호
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• pp.2865-2870
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• 2013

Ni-Ag core-shell nanoparticles were synthesized by polyol process and microemulsion technique successfully. In the polyol process, a chemical reduction method for preparing highly dispersed pure nickel and Ag shell formation have been reported. The approach involved the control of reaction temperature and reaction time in presence of organic solvent (ethylene glycol) as a reducing agent for Ag cation with poly(vinyl-pyrrolidone) (PVP. Mw = 40000) as a capping agent. In microemulsion method, the emulsion was prepared by water/cetyltrimetylammonium bromide (CTAB)/cyclohexane. The size of microemulsion droplet was determined by the molar ratio of water to surfactant (${\omega}_o$). The core-shell formation along with the change in structural phase and stability against oxidation at high temperature heat treatments of nanoparticles were investigated by X-ray diffraction and TEM analysis. Under optimum conditions the polyol process gives the Ni-Ag core-shell structures with 13 nm Ni core covered with 3 nm Ag shell, while the microemulsion method gives Ni core diameter of 8 nm with Ag shell of thickness 6 nm. The synthesized Ni-Ag core-shell nanoparticles were stable against oxidation up to $300^{\circ}C$.

• Restorative Dentistry and Endodontics
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• 제9권1호
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• pp.81-87
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• 1983

The purpose of this study was to observe and identify the phases of amalgam and to know the transformation of microstructure in the set amalgam by lapse of time. In this study, shofu spherical-D alloy was used. After trituration of amalgam alloy and mercury (Wig-L-Bug), it was filled in the stone dies. This specimens being polished and etched by usual method was observed under optical microscope using metallurgical microscope. And then X-ray diffractometer was used to analyze the phases contents and transformation of microstructure at $2{\frac{1}{2}}$ hours, 15 hours, 28 hours and 2 years after being amalgamated. The following results were obtained: 1. Shofu spherical-D alloy powder was composed of ${\gamma}$ phase, ${\epsilon}$phase and Ag-Cu eutectic phases. 2. ${\gamma}_2$ phases were appeared at $2{\theta}$ values ($32.0^{\circ}$ and $43.8^{\circ}$) in the amalgam which was analyzed at $2{\frac{1}{2}}$ hours and 15 hours after trituration with mercury. 3. In the amalgam at 28 hours, ${\gamma}_2$ phase was found at $2{\theta}$ value ($43.8^{\circ}$) at 35 hour, $r_2$ phase was appeared at $2{\theta}$ value $32.0^{\circ}$. 4. No ${\gamma}_2$ phases were observed in the 2 years old amalgam. But ${\eta}$ ($Cu_6Sn_5$) phases were found at $2{\eta}$ values $29.4^{\circ}$ and $42.4^{\circ}$.

• Bulletin of the Korean Chemical Society
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• 제33권4호
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• pp.1279-1284
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• 2012

Silica supported $Cs_{2.5}H_{0.5}PMo_{12}O_{40}$ catalyst was prepared through sol-gel method with ethyl silicate-40 as silicon resource and characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy, nitrogen adsorption-desorption and potentiometric titration methods. The $Cs_{2.5}H_{0.5}PMo_{12}O_{40}$ particles with Keggin-type structure well dispersed on the surface of silica, and the catalyst exhibited high surface area and acidity. The catalytic performance of the catalysts for benzene liquid-phase nitration was examined with 65% nitric acid as nitrating agent, and the effects of various parameters were tested, which including temperature, time and amount of catalyst, reactants ratio, especially the recycle of catalyst was emphasized. Benzene was effectively nitrated to mononitro-benzene with high conversion (95%) in optimized conditions. Most importantly, the supported catalyst was proved has excellent stability in the nitration progress, and there were no any other organic solvent and sulfuric acid were used in the reaction system, so the liquid-phase nitration of benzene that we developed was an eco-friendly and attractive alternative for the commercial technology.

• Corrosion Science and Technology
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• 제8권4호
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• pp.143-147
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• 2009

In biomedical implants and dental fields, titanium has been widely utilized for excellent corrosion resistance and biocompatibility. However, Ti and its alloys are nonbioactive after being implanted in bone. In this study, for the purpose of improvement in biocompatibility the anodic $TiO_2$ layer on Ti-xNb alloys were fabricated by electrochemical method in phosphate solution, and the effect of Nb content on the pore size, the morphology and crystallinity of Ti oxide layer formed by the anodic oxidation method was investigated. The Ti containing Nb up to 3 wt%, 20 wt% and 40 wt% were melted by using a vacuum furnace. The sample were cut, polished, and homogenized for 24 hr at $1050^{\circ}C$ for surface roughness test and anodizing. Titanium anodic layer was formed on the specimen surface in an electrolytic solution of 1 M phosphoric acid at constant current densities ($30mA/cm^2$) by anodizing method. Microstructural morphology, crystallinity, composition, and surface roughness of oxide layer were observed by FE-SEM, XRD, EDS, and roughness tester, respectively. The structure of alloy was changed from $\alpha$-phase to $\beta$-phase with increase of Nb content. From XRD results, the structure of $TiO_2$ formed on the Ti-xNb surface was anatase, and no peaks of $Nb_2O_5$ or other Nb oxide were detected suggesting that Nb atoms are dispersed in $TiO_2$-based solid solution. Surface roughness test and SEM results, pore size formed on surface and surface roughness decreased as Nb content increased. From the line analysis results, intensity of Ti peak was high in the center of pore, whereas, intensity of O peak was high in the outside of pore center.

• Membrane and Water Treatment
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• 제7권3호
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• pp.175-191
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• 2016

In this work, oil-in-water emulsions (O/W) were prepared successfully by membrane emulsification with $0.5{\mu}m$ pore size membrane. Sunflower oil was emulsified in aqueous Tween80 solution with a simple crossflow apparatus equipped with ceramic tube membrane. In order to increase the shear-stress near the membrane wall, a helical-shaped reducer was installed within the lumen side of the tube membrane. This method allows the reduction of continuous phase flow and the increase of dispersed phase flux, for cost effective production. Results were compared with the conventional cross-flow membrane emulsification method. Monodisperse O/W emulsions were obtained using tubular membrane with droplet size in the range $3.3-4.6{\mu}m$ corresponded to the membrane pore diameter of $0.5{\mu}m$. The final aim of this study is to obtain O/W emulsions by simple membrane emulsification method without reducer and compare the results obtained by membrane equipped with helix shaped reducer. To indicate the results statistical methods, $3^p$ type full factorial experimental designs were evaluated, using software called STATISTICA. For prediction of the flux, droplet size and PDI a mathematical model was set up which can describe well the dependent variables in the studied range, namely the run of the flux and the mean droplet diameter and the effects of operating parameters. The results suggested that polynomial model is adequate for representation of selected responses.

• 한국재료학회지
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• 제17권1호
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• pp.11-17
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• 2007

Turbulent in-situ mixing process is a new material process technology to get dispersed phase in nanometer size by controlling reaction of liquid/solid, liquid/gas, flow ana solidification speed simultaneously. In this study, mixing which is the key technology to this synthesis method was studied by computational fluid dynamics. For the simulation of mixing of liquid metal, static mixers investigated. Two inlets for different liquid metal meet ana merge like 'Y' shape tube having various shapes and radios of curve. The performance of mixer was evaluated with quantitative analysis with coefficient of variance of mass fraction. Also, detailed plots of intersection were presented to understand effect of mixer shape on mixing. The simulations show that the Reynolds number (Re) is the important factor to mixing and dispersion of $TiB_2$ particles. Mixer was designed according to the simulation, and $Cu-TiB_2$ nano composites were evaluated. $TiB_2$ nano particles were uniformly dispersed when Re was 1000, and cluster formation and reduction in volume fraction of $TiB_2$ were found at higher Re.

• 한국분말재료학회지
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• 제16권6호
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• pp.389-395
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• 2009

A Si-CuO-graphite composite was prepared by a mechanical alloying (MA) method. The Si-CuO composite has a mixture structure, where CuO is homogeneously dispersed in Si. Also, $Cu_2O$ and $Cu_3Si$ phases were formed during MA and heat treatment. Graphite with the Si-CuO composite was mixed in the same mill for 30 minutes with weight ratio of Si-CuO composite and graphite as 1:1. The Si-CuO composite was homogeneously covered with graphite. SiC phase was not formed. Electrochemical tests of the composite have been investigated, and the first charge and discharge capacities of the material were about 870mAh/g and 660mAh/g, respectively. Those values are about 76% of the first cycle efficiency. The cycle life of the composite showed that the initial discharge capacity of 660 mAh/g could be maintained up to 92% after 20 cycles.

• 열처리공학회지
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• 제9권2호
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• pp.121-129
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• 1996

The solubility of Ti in Al matrix was determined by X-ray diffraction method on two different mechanical alloying systems, i.e Al+$Al_3Ti$ and Al+Ti alloys. Starting powder compositions of two systems were chosen for final volume fraction of $Al_3Ti$ phase being 25%. The solubility of Ti in ${\alpha}$-Al was estimated by the lattice parameter measurement of Al. For Al+$Al_3Ti$ mixture, it appeared that some of $Al_3Ti$ particles decomposed during milling and maximum solubility of Ti in Al was about 0.99%. The majority of $Al_3Ti$ particles were dispersed uniformly in Al matrix, having approximate size of 100~200 nm. On the other hand, higher Ti solubility of 1.24 wt.% was found in Al+Ti system, with starting composition of Al+10 wt.%Ti. After 15 hours of milling, Ti phase was identified as 20 nm sized particles embedded in Al matrix. The annealing of mechanically alloyed powders from Al+$Al_3Ti$ and Al+10 wt.%Ti systems was followed in the temperature range of 200 to $600^{\circ}C$ to study thermal stability of supersaturated solution of Al(Ti). After annealing, the lattice parameter of Al reverted back to that of pure Al, and the peak intensity ratio of $Al_3Ti$/Al was increased more than the original value before annealing. These results suggest that Ti dissolve into alpha-Al solutions during milling, and by annealing, $Do_{22}-Al_3Ti$ phase forms from Al(Ti) solution.