• Journal of the Korean Ceramic Society
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• v.40 no.6
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• pp.577-582
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• 2003

BaTiO$_3$ fine powders were synthesized by hydrothermal process from peroxo-coprecipitate precursors. The peroxo-coprecipitates were obtained by addition of the BaCl$_2$, TiCl$_4$, and $H_2O$$_2$ aqueous solution to an ammonium solution. Hydrothermal reaction was conducted at various reaction temperatures, times and pH ranges. Unlike the conventional hydrothermal synthesis which needs highly alkaline condition over pH 13 with KOH or NaOH, the present method offered well-developed crystalline (perovskite) BaTiO$_3$ powders synthesized below pH 12 with use of ammonium solution. It was found that the phase-pure fine powders were formed at temperatures as low as 11$0^{\circ}C$ and the properties of the powders synthesized over 13$0^{\circ}C$ were almost same regardless of the reaction time. BET surface area of the prepared powder was as high as 76 $m^2$/g and the calculated particle (particulate) size was below 20 nm. The ultrafine particulates formed weak agglomerates. The microstructure and dielectric properties of BaTiO$_3$ ceramics sintered at the temperature range of 1150~125$0^{\circ}C$ were evaluated.

• Journal of dental hygiene science
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• v.17 no.4
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• pp.358-367
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• 2017

The purpose of this study was to evaluate the influence of water infiltration and flexural strength changes in dental porcelain with glazing treatment. The block specimens were prepared as experimental materials, using feldspar type commercial dental porcelain; then, these were fired at $940^{\circ}C$ for 1 minute. The fired specimens were polished with a dimension of $40{\times}5.5{\times}5mm$. The specimens were distributed to two experimental groups: with and without glazing treatment specimens (n=5), and they were immersed in a solution of pH 7 for 3, 7, and 20 days at $40^{\circ}C$ after fabrication. To evaluate the flexural strength changes with water infiltration treatment in specimens with and without glazing, the 3-point flexural test was performed, using a universal testing machine until failure occurred. Starting powder and fired specimens consisted of amorphous and leucite crystalline phase. The Vickers hardness of fired specimens was more than 1.6 times higher than that of the enamel of natural teeth. According to porosimeter results, the specimens without glazing treatment exhibited a porosity of about 14.7%, whereas the glazed specimens exhibited the lowest porosity at about 1.1%. The average flexural strength of glazed specimens was higher than the flexural strength of specimens without glazing treatment (p<0.05). The flexural strength of all specimens with and without glazing treatment deteriorated with accelerated aging in the solution. In addition, significant differences between these two treatment groups were observed in all of the specimens treated at various water infiltration periods (p<0.05). The exposure of internal pores and micro-cracks in the surface due to polishing of the fired specimens influenced mechanical behaviors. Especially, the flexural strength in specimens without glazing treatment has shown significant degradation with the infiltration of water. Therefore, this study suggests that glazing processes can improve mechanical properties of dental porcelain.

• Journal of the Korean Ceramic Society
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• v.39 no.8
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• pp.789-794
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• 2002

In this study, nano-sized Si-C-N precursor powders were synthesized by Chemical Vapor Condensation Method(CVC) using TMS(Tetramethylsilane: $Si(CH_3)_4$), $NH_3$ and $H_2$ gases under the various reaction conditions of the reaction temperature, TMS/$NH_3$ ratio and TMS/$H_2$ ratio. XRD and FESEM were used to analysis the crystalline phase and the average particle size of the synthesized powders. It was found that the obtained powders under the considering conditions were all spherical amorphous powder with the particle size of 87∼130 nm. The particle size was decreased as the reaction temperature increased and TMS/$NH_3$ and TMS/$H_2$ ratio decreased. As the results of EA analysis, it was found that the synthesized powders had been formed the powders composed of Si, N, C and H. Through FT-IR results, it was found that the synthesized powders were Si-C-N precursor powders with Si-C, Si-N and C-N bonds.

• Journal of the Korean Ceramic Society
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• v.39 no.8
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• pp.783-788
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• 2002

In this study, nano-sized Si-C-N precursor powders were synthesized by Chemical Vapor Condensation Method(CVC) using TMS(Tetramethylsilane: Si($CH_3)_4$), $NH_3$ and $H_2$ gases under the various reaction conditions of the reaction temperature, TMS/$NH_3$ ratio and TMS/$H_2$ ratio. XRD and FESEM were used to analysis the crystalline phase and the average particle size of the synthesized powders. It was found that the obtained powders under the considering conditions were all spherical amorphous powder with the particle size of 87∼130 nm. The particle size was decreased as the reaction temperature increased and TMS/$NH_3$ and TMS/$H_2$ ratio decreased. As the results of EA analysis, it was found that the synthesized powders had been formed the powders composed of Si, N, C and H. Through FT-IR results, it was found that the synthesized powders were Si-C-N precursor powders with Si-C, Si-N and C-N bonds.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.183-183
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• 2014

Recently, multiferroic materials gain much attention due to their fascinating fundamental physical properties. These materials offer wide range of potential applications such as data storage, spintronic devices and sensors, where both electronic and magnetic polarizations can be coupled. Among single-phase multiferroic materials, $BiFeO_3$ is typical because of the room-temperature magnetoelectric coupling in view of long-range magnetic- and ferroelectric-ordering temperatures. However, $BiFeO_3$ is well known to have large leakage current and small spontaneous polarization due to the existence of oxygen vacancies and other defects. Furthermore the magnetic moment of pure $BiFeO_3$ is very weak owing to its antiferromagnetic nature. Recently, various attempts have been performed to improve the multiferroic properties of $BiFeO_3$ through the co-doping at the A and the B sites, by making use of the fact that the intrinsic polarization and magnetization are associated with the lone pair of $Bi^{3+}$ ions at the A sites and the partially-filled 3d orbitals of $Fe^{3+}$ ions at the B sites, respectively. In this study, $BiFeO_3$, $Bi_{0.9}Ho_{0.1}FeO_3$, $BiFe_{0.97}Ni_{0.03}O_3$ and $Bi_{0.9}Ho_{0.1}Fe_{0.97}Ni_{0.03}O_3$ bulk compounds were prepared by solid-state reaction and rapid sintering. High-purity $Bi_2O_3$, $Ho_2O_3$, $Fe_2O_3$ and $NiO_2$ powders with the stoichiometric proportions were mixed, and calcined at $500^{\circ}C$ for 24 h to produce the samples. The samples were immediately put into an oven, which was heated up to $800^{\circ}C$ and sintered in air for 1 h. The crystalline structure of samples was investigated at room temperature by using a Rigaku Miniflex powder diffractometer. The field-dependent and temperature-dependent magnetization measurements were performed with a vibrating-sample magnetometer and superconducting quantum-interference device.

• Journal of the Mineralogical Society of Korea
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• v.31 no.1
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• pp.23-32
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• 2018

Noerok ia a green pigment used in Joseon dynasty, and its main usage was for forming foundation layers of Dancheong, the ornamental paintings on the surface of traditional buildings in Korea, such as the Daeung-jeon(main hall) of Bulguk-sa temple. In this research, we investigated the mineralogical characteristic changes of Noerok, a traditional Korean pigment, depending on its firing temperature. The Noerok that we experimented on was mined from Noeseong Mountain, Pohang where it is locally reserved. The major composition mineral is Celadonite, and the main constituent elements are Fe, Si, K and Mg, that refers to the existence of Fe-rich mica. As a result of phased firing experiment from $105^{\circ}C$ to $1000^{\circ}C$, the color was changed from green to pale green, then to brown, and finally to red in order. In the thermal analysis, endothermic reaction induced by the dehydration of crystalline water was confirmed at around $616^{\circ}C$. In the mineralogical change, the crystal surface [($11{\bar{1}}$) and ($02{\bar{1}}$)] of the mineral collapsed at temperatures above $600^{\circ}C$, and iron oxide was formed at $1000^{\circ}C$ or higher. Therefore, it is estimated that the crystallization temperature of Noerok is below $600^{\circ}C$, and it is also considered that it has undergone the alteration phase up to stage I, based on the presence of only a celadonite.

• Resources Recycling
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• v.18 no.4
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• pp.24-30
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• 2009

Rare earth based calcium aluminate phosphor ($CaAl_2O_4:Eu^{2+}$, $Nd^{3+}$) supported $TiO_2$ nanoparticles are synthesized by using sol-gel method, which are further characterized using powder X-ray diffraction (XRD), fourier transform infrared (FT-IR), diffuse reflectance UV-Visible spectroscopy (DRS UV-Vis) and transmission electron microscopy (TEM). The XRD pattern of as-prepared and sintered phosphor supported $TiO_2$ does not show the tendency to change the crystal structure from anatase to rutile phase up to $600^{\circ}C$. This indicates that the phosphor support might inhibit the densification and crystallite growth by providing dissimilar boundaries. The diffuse reflectance spectral (DRS) measurements showed shift towards longer wavelength indicating reduction in the band-gap energy as compared to free $TiO_2$. The FT-IR spectra of phosphor supported $TiO_2$ nanoparticles show shift in the peak positions to lower wavelengths. This indicates that the $TiO_2$ nanoparticles are not free, but covalently bonded to the phosphor support. TEM micrographs show presence of crystalline and spherical $TiO_2$ nanoparticles (8 - 15 nm diameter) dispersed uniformly on the surface of phosphor.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.250-250
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• 2012

Recently, multiferroic materials have attracted much attention due to their fascinating fundamental physical properties and potential technological applications in magnetic/ferroelectric data storage systems, quantum electromagnets, spintronics, and sensor devices. Among single-phase multiferroic materials, $BiFeO_3$, in particular, has received considerable attention because of its very interesting magnetoelectric properties for application to spintronics. Enhanced ferromagnetism was found by Fe-site ion substitution with magnetic ions. In this study, $BiFe_{1-x}Ni_xO_3$ (x=0 and 0.05) bulk ceramic compounds were prepared by solid-state reaction and rapid sintering. High-purity $Bi_2O_3$, $Fe_3O_4$ and NiO powders were mixed with the stoichiometric proportions, and calcined at $450^{\circ}C$ for 24 h to produce $BiFe_{1-x}Ni_xO_3$. Then, the samples were directly put into the oven, which was heated up to $800^{\circ}C$ and sintered in air for 20 min. The crystalline structure of samples was investigated at room temperature by using a Rigaku Miniflex powder diffractometer. The Raman measurements were carried out with a Raman spectrometer with 514.5-nm-excitation Ar+-laser source under air ambient condition on a focused area of $1-{\mu}m$ diameter. The field-dependent magnetization and the temperature-dependent magnetization measurements were performed with a vibrating-sample magnetometer. The x-ray diffraction study demonstrates the compressive stress due to Ni substitution at the Fe site. $BiFe_{0.95}Ni_{0.05}O_3$ exhibits the rhombohedral perovskite structure R3c, similar to $BiFeO_3$. The lattice constant of $BiFe_{0.95}Ni_{0.05}O_3$ is smaller than of $BiFeO_3$ because of the smaller ionic radius of Ni3+ than that of Fe3+. The field-dependent magnetization of $BiFe_{0.95}Ni_{0.05}O_3$ exhibits a clear hysteresis loop at 300 K. The magnetic properties of $BiFe_{0.95}Ni_{0.05}O_3$ were improved at room temperature because of the existence of structurally compressive stress.

• Proceedings of the Materials Research Society of Korea Conference
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• 2012.05a
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• pp.65-65
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• 2012

Copper zinc tin sulfide ($Cu_2ZnSnS_4$, CZTS) is a very promising material as a low cost absorber alternative to other chalcopyrite-type semiconductors based on Ga or In because of the abundant and economical elements. In addition, CZTS has a band-gap energy of 1.4~1.5eV and large absorption coefficient over ${\sim}10^4cm^{-1}$, which is similar to those of $Cu(In,Ga)Se_2$(CIGS) regarded as one of the most successful absorber materials for high efficient solar cell. Most previous works on the fabrication of CZTS thin films were based on the vacuum deposition such as thermal evaporation and RF magnetron sputtering. Although the vacuum deposition has been widely adopted, it is quite expensive and complicated. In this regard, the solution processes such as sol-gel method, nanocrystal dispersion and hybrid slurry method have been developed for easy and cost-effective fabrication of CZTS film. Among these methods, the hybrid slurry method is favorable to make high crystalline and dense absorber layer. However, this method has the demerit using the toxic and explosive hydrazine solvent, which has severe limitation for common use. With these considerations, it is highly desirable to develop a robust, easily scalable and relatively safe solution-based process for the fabrication of a high quality CZTS absorber layer. Here, we demonstrate the fabrication of a high quality CZTS absorber layer with a thickness of 1.5~2.0 ${\mu}m$ and micrometer-scaled grains using two different non-vacuum approaches. The first solution-processing approach includes air-stable non-toxic solvent-based inks in which the commercially available precursor nanoparticles are dispersed in ethanol. Our readily achievable air-stable precursor ink, without the involvement of complex particle synthesis, high toxic solvents, or organic additives, facilitates a convenient method to fabricate a high quality CZTS absorber layer with uniform surface composition and across the film depth when annealed at $530^{\circ}C$. The conversion efficiency and fill factor for the non-toxic ink based solar cells are 5.14% and 52.8%, respectively. The other method is based on the nanocrystal dispersions that are a key ingredient in the deposition of thermally annealed absorber layers. We report a facile synthetic method to produce phase-pure CZTS nanocrystals capped with less toxic and more easily removable ligands. The resulting CZTS nanoparticle dispersion enables us to fabricate uniform, crack-free absorber layer onto Mo-coated soda-lime glass at $500^{\circ}C$, which exhibits a robust and reproducible photovoltaic response. Our simple and less-toxic approach for the fabrication of CZTS layer, reported here, will be the first step in realizing the low-cost solution-processed CZTS solar cell with high efficiency.

• Korean Journal of Materials Research
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• v.11 no.5
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• pp.405-412
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• 2001

Corrosion tests were carried out in $360^{\circ}C$ water and $360^{\circ}C$ 70ppm LiOH solution to investigate the corrosion behavior of new zirconium alloys (Zr-0.4Nb-0.8Sn-xFeCrMn, Zr-0.2Nb-1.1Sn-xFeCrMn, Zr-1.0Nb-xFeCu). Microstructures of tested alloys were analyzed by optical microscope and TEM. The cross-sectional surface and crystalline structure of the oxide layer were analyzed by SEM and XRD. From the results of corrosion test, all the alloys showed higher corrosion rates in $360^{\circ}C$ 70ppm LiOH aqueous solution thats in $360^{\circ}C$ water. Especially, high Nb-containing alloy exhibited the acceleration of corrosion rate in LiOH solution. The low Nb- and Sn-added alloys showed better corrosion resistance than the Sn- free high Nb alloy. from the effect of final annealing on the corrosion, it was observed that the partially recrystallized alloys showed better corrosion resistance than fully recrystallized alloys. This would be related to the size and distribution of the second phase particles.