• Journal of the Korea Academia-Industrial cooperation Society
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• v.22 no.4
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• pp.413-418
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• 2021

Nano-materials with high effective surface areas have been applied to functional materials, such as high sensitive gas sensors and biosensors and high-efficiency catalytic materials. In this study, titanate sheets with a 3D nano-wall-like structure, high effective surface area, were synthesized vertically to the substrate by a chemical bath deposition (CBD) process using a Ti sheet and urea. The synthesis temperature and synthesis duration time were controlled to the optimal conditions of a 3D nano-wall-like structure in the CBD process. The synthesized ammonium titanate sheets with a 3D nano-wall-like structure were annealed in air to transform to TiO2 with a 3D nano-wall-like structure for various applications. As a result, the optimal temperature in the CBD process for the synthesis of a uniform ammonium titanate sheet with a 3D nano-wall-like structure was 90 ℃. TiO2 with a 3D nano-wall-like structure was obtained from the ammonium titanate sheet with a 3D nano-wall-like structure by annealing above 550 ℃ for three hours. In particular, TiO2 with a 3D nano-wall-like structure with a dominant rutile phase was obtained by post-annealing at 700 ℃. On the other hand, damage to the 3D nano-wall edge was observed after 700 ℃ post-annealing.

• Korean Journal of Materials Research
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• v.17 no.1
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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.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.33 no.5
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• pp.373-379
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• 2020

In this study, TiN-coated cBN (cubic-structure boron nitride) powders were successfully synthesized by a sol-gel method using titanium (IV) isopropoxide (TTIP) and by controlling the heat treatment conditions. After the sol-gel process, amorphous nano-sized TiO_x was uniformly coated on the surface of cBN powder particles. The obtained TiO_x-coated cBN powders were heated at 1,000~1,300℃ for 1 or 6 h in a flow of 95%N₂-5%H₂ mixed gas. With increasing temperature, the chemical composition of the TiO_x coating layer changed in the order of TiO₂→Ti₆O₁₁→Ti₄O₇→TiN due to reduction of the Ti ions. The TiN coating layer was observable in the samples heated at 1,200℃ and appeared as the main phase in the sample heated at 1,300℃. The resulting thickness of the TiN coating layer of the sample heated at 1,300℃ was approximately 45~50 nm.

• Korean Journal of Materials Research
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• v.21 no.8
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• pp.468-475
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• 2011

[ $LaMeO_3$ ](Me = Cr, Co) powders were prepared using the polymeric precursor method. The effects of the chelating agent and the polymeric additive on the synthesis of the $LaMeO_3$ perovskite were studied. The samples were synthesized using ethylene glycol (EG) as the solvent, acetyl acetone (AcAc) as the chelating agent, and polyvinylpyrrolidone (PVP) as the polymer additive. The thermal decomposition behavior of the precursor powder was characterized using a thermal analysis (TG-DTA). The crystallization and particle sizes of the $LaMeO_3$ powders were investigated via powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and particle size analyzer, respectively. The as-prepared precursor primarily has $LaMeO_3$ at the optimum condition, i.e. for a molar ratio of both metal-source (a : a) : EG (80a : 80a) : AcAc (8a) inclusive of 1 wt% PVP. When the as-prepared precursor was calcined at $700^{\circ}C$, only a single phase was observed to correspond with the orthorhombic structure of $LaCrO_3$ and the rhombohedral structure of $LaCoO_3$. A solid-electrolyte impedance-metric sensor device composed of $Li_{1.5}Al_{0.5}Ti_{1.5}(PO_4)_3$ as a transducer and $LaMeO_3$ as a receptor has been systematically investigated for the detection of NOx in the range of 20 to 250 ppm at $400^{\circ}C$. The sensor responses were able to divide the component between resistance and capacitance. The impedance-metric sensor for the NO showed higher sensitivity compared with $NO_2$. The responses of the impedance-metric sensor device showed dependence on each value of the NOx concentration.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.08a
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• pp.281-281
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• 2010

Very low refractive index (<1.4) materials have been proved to be the key factor improving the performance of various optical components, such as reflectors, filters, photonic crystals, LEDs, and solar cell. Highly porous SiO2 are logically designed for ultralow refractive index materials because of the direct relation between porosity and index of refraction. Among them, ordered macroporous SiO2 is of potential material since their theoretically low refractive index ~1.10. However, in the conventional synthesis of ordered macroporous SiO2, the time required for the crystallization of organic nanoparticles, such as polystyrene (PS), from colloidal solution into well ordered template is typical long (several days for 1 cm substrate) due to the low interaction between particles and particle - substrate. In this study, polystyrene - polyacrylic acid (PS-AA) nanoparticles synthesized by miniemulsion polymerization method have hydrophilic polyacrylic acid tails on the surface of particles which increase the interaction between particle and with substrate giving rise to the formation of PS-AA film by simply spin - coating method. Less ordered with controlled thickness films of PS-AA on silicon wafer were successfully fabricated by changing the spinning speed or concentration of colloidal solution, as confirmed by FE-SEM. Based on these template films, a series of macroporous SiO2 films whose thicknesses varied from 300nm to ~1000nm were fabricated either by conventional sol - gel infiltration or gas phase deposition followed by thermal removal of organic template. Formations of SiO2 films consist of interconnected air balls with size ~100 nm were confirmed by FE-SEM and TEM. These highly porous SiO2 show very low refractive indices (<1.18) over a wide range of wavelength (from 200 to 1000nm) as shown by SE measurement. Refraction indices of SiO2 films at 633nm reported here are of ~1.10 which, to our best knowledge, are among the lowest values having been announced.

• Applied Chemistry for Engineering
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• v.10 no.8
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• pp.1210-1215
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• 1999

Optimum conditions of the hydrogenation of PNA to pure PPD were determined in a three-phase slurry reactor with suspended Pd/C catalyst particles. Minimization of mass transfer resistances at the interfaces of both gas-liquid and liquid-catalyst particles and control of overall reaction rate on catalyst surface leaded to decrease the hydrogen starvation on reaction active sites and to reduce the side reactions during hydrogenation. The optimum temperature, pressure, and catalysst concentration were confirmed to be in the range of $60^{\circ}C$, 60~70 psig, and 1~2 g-cat/L, respectively. Reaction rate was zero order with respect to the concentration of PNA and 1st order with respect to the pressure of hydrogen(P). Overall rate expression of the reaction was $R_A=6.44{\times}10^6{\cdot}H{\cdot}P{\cdot}m{\cdot}$exp(-4659/T) where H is constant, m is concentration of catalyst, and T is temperature.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.9 no.5
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• pp.516-520
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• 1999

Mechanical alloying (MA) by planetary type ball mill of pure iron powders was carried out under the ammonia gas atmosphere. The powders of metastable iron nitrides was synthesized up to the nitrogen content of 23 at% N. The observed phases are identified as the super-saturated bcc solid solution for the nitrogen concentration below 14.5 at% N and the non-equilibrium hcp phase stable at high temperature for 20.8 at.% N. Magnetization of Fe-N powders gradually decreases with increasing the N concentration on contrast to the enhancement reported for the bct iron nitrides. Neutron diffraction experiments also provide detailed information concerning the local atomic structure surrounding the nitrogen atoms. The coordination number of Fe atom around a nitrogen atom for the iron nitride containing 9.5 at% N turns out to be 3.9 atoms. This suggests that a nitrogen atom is situated at a center of the tetrahedron formed by iron atoms.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.18 no.1
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• pp.27-32
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• 2008

Novel long persistent phosphors of $CaZrO_3:Er^{3+}$ have been synthesized by traditional solid state reaction method. The long persistent phosphor crystalline particles were characterized by the X-ray diffraction (XRD), photoluminescence spectrophotometer, thermoluminescence (TL) and luminance meter. The results reveal that the samples are composed of single $CaZrO_3$ phase. The broadband emission spectra of 446 nm peak and 550 nm peak was revealed by synthesized at high temperature in $N_2$ gas. Green long persistent phosphors have been observed in the sys_em for over 6 h after UV irradiation (254 nm). The main emission peak was ascribed to $Er^{3+}$ ions transition from $^5D_{5/2}{\rightarrow}^4F_{9/2},\;^2H_{12/2},\;^4S_{3/2}{\rightarrow}^4I_{13/2}\;and\;^2G_{9/2}{\rightarrow}^4I_{13/2}$, and the afterglow may be ascribed to the suitable trap centers in the $CaZrO_3$ host lattice.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.6 no.4
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• pp.509-520
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• 1996

Ultrafine calcim carbonate powders with the size of $0.05~0.1\;{\mu}m$ and the calcite phase were synthesized by the nozzle spouting method, which could be only obtained when high calcium ion concentration within slurry was maintained at the beginning of the reaction. But, in the regions of low ${Ca(OH)}_2$ concentration (0.5~1.0 wt%) or high ${Ca(OH)}_2$ concentration (<3.0 wt%), synthesized calcium carbonate powder was shown the large particle size with agglomeration. To obtain ultrafine calcium carbonate powder in this region, the methods of slurry circuation and $CO_{2}$ gas supply were changed during reaction. Resultly, it was possible to synthesize ultrafine particles (${\approx}0.05{\mu}\textrm{m}$)in the regions of low ${Ca(OH)}_2$ concentration (${\approx}0.5wt%$) and high ${Ca(OH)}_2$ concentration (${\approx}0.5wt%$), which can not be obtained the fine calcium carbonate powder still now.

• Nuclear Engineering and Technology
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• v.52 no.5
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• pp.1013-1021
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• 2020

A combination of simultaneous thermal analysis, evolved gas analysis and non-ambient XRD techniques was used to characterise and investigate the conversion reactions of ammonium uranates into uranium oxides. Two solid phases of the ternary system NH₃ - UO₃ - H₂O were synthesised under specified conditions. Microspheres prepared by the sol-gel method via internal gelation were identified as 3UO₃·2NH₃·4H₂O, whereas the product of a typical ammonium diuranate precipitation reaction was associated to the composition 3UO₃·NH₃·5H₂O. The thermal decomposition profile of both compounds in air feature distinct reaction steps towards the conversion to U₃O₈, owing to the successive release of water and ammonia molecules. Both compounds are converted into α-U₃O₈ above 550 ℃, but the crystallographic transition occurs differently. In compound 3UO₃·NH₃·5H₂O (ADU) the transformation occurs via the crystalline β-UO₃ phase, whereas in compound 3UO₃·2NH₃·4H₂O (microspheres) an amorphous UO₃ intermediate was observed. The new insights obtained on these uranate systems improve the information base for designing and synthesising minor actinide-containing target materials in future applications.