• Korean Journal of Materials Research
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• v.19 no.8
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• pp.412-416
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• 2009

In this study, 3 mol% yttria-tetragonal zirconia polycrystal (3Y-TZP) nanoparticles were synthesized by the glycothermal method under various reaction temperatures and times. The co-precipitated precursor of 3Y-TZP was prepared by adding $NH_4OH$ to starting solutions, and then the mixtures were placed in an autoclave reactor. Tetragonal yttria-doped zirconia nanoparticles were afforded through a glycothermal reaction at a temperature as low as $220^{\circ}C$, using co-precipitated gels of $ZrCl_4$ and $YCl_3{\cdot}6H_2O$ as precursors and 1,4-butanediol as the solvent. The synthesized 3Y-TZP particles were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Raman spectroscopy. The 3Y-TZP particles have a stable tetragonal phase only at glycothermal temperatures above $200^{\circ}C$. To investigate phase transition, the 3Y-TZP particles were heat treated from 400 to $1400^{\circ}C$ for 2 h. Raman analysis indicated that, after heat treatment, the tetragonal phase of the 3Y-TZP particles remained stable. The results of this study, therefore, suggest that 3Y-TZP powders can be prepared by the glycothermal method.

• Journal of the Korean Ceramic Society
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• v.39 no.7
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• pp.642-648
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• 2002

Barium Titanate(BaTiO$_3$) nanoparticles were prepared at 22$0^{\circ}C$ through glycothermal process by using barium hydroxide and amorphous titanium hydrous gel as precursor and 1,4-butanediol and distilled water as solvent. It is demonstrated that the size of BaTiO$_3$ particles can be controlled by reaction conditions such as various content of 1,4-butanediol/distilled water volume ratio. This processing method can fabricate BaTiO$_3$ powders, which have a narrow distribution and exhibit good dispersion. The particle size of BaTiO$_3$ powders obtained by glycothermal process were about 50 nm to 200 nm on the condition that reaction temperature was 22$0^{\circ}C$ and holding time was 24 h.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.06a
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• pp.167-168
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• 2009

Phase pure barium magnesium tantalate $Ba(Mg_{1/3}Ta_{2/3})O_3$(BMT) nanopowders were synthesized at temperature as low as $220^{\circ}C$ through glycothermal reaction by using $Ba(OH)_2{\cdot}8H_2O$, $Mg(NO_3){\cdot}6H_2O$, and $TaCl_5$ as precursors and 1,4-butandiol as solvent. XRD, SEM, and TGA data support that glycothermal processing method provides a simple low temperature route for producing fine grained BMT nanopowders without alkaline mineralizers. BMT nanopowders synthesized at $220^{\circ}C$ showed more homogenous with rounded morphologies.

• Proceedings of the Korean Ceranic Society Conference
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• 2003.10a
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• pp.169.2-169
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• 2003

• Korean Journal of Materials Research
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• v.27 no.9
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• pp.489-494
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• 2017

ZnS powder was synthesized using a relatively facile and convenient glycothermal method at various reaction temperatures. ZnS was successfully synthesized at temperatures as low as $125^{\circ}C$ using zinc acetate and thiourea as raw materials, and diethylene glycol as the solvent. No mineralizers or precipitation processes were used in the fabrication, which suggests that the spherical ZnS powders were directly prepared in the glycothermal method. The phase composition, morphology, and optical properties of the prepared ZnS powders were characterized using XRD, FE-SEM, and UV-vis measurements. The prepared ZnS powders had a zinc blende structure and showed average primary particles with diameters of approximately 20~30 nm, calculated from the XRD peak width. All of the powders consisted of aggregated secondary powders with spherical morphology and a size of approximately $0.1{\sim}0.5{\mu}m$; these powders contained many small primary nanopowders. The as-prepared ZnS exhibited strong photo absorption in the UV region, and a red-shift in the optical absorption spectra due to the improvement in powder size and crystallinity with increasing reaction temperature. The effects of the reaction temperature on the photocatalytic properties of the ZnS powders were investigated. The photocatalytic properties of the as-synthesized ZnS powders were evaluated according to the removal degree of methyl orange (MO) under UV irradiation (${\lambda}=365nm$). It was found that the ZnS powder prepared at above $175^{\circ}C$ exhibited the highest photocatalytic degradation, with nearly 95 % of MO decomposed through the mediation of photo-generated hydroxyl radicals after irradiation for 60 min. These results suggest that the ZnS powders could potentially be applicable as photocatalysts for the efficient degradation of organic pollutants.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2006.06a
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• pp.286-287
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• 2006

Barium titanate ($BaTiO_3$) glycolate particles were synthesized at temperature as low as $100^{\circ}C$ through glycothermal reaction by using $Ba(OH)_2{\cdot}8H_2O$ and amorphous titanium hydrous gel as precursors and ethylene glycol as solvent. The particle size and morphology of $BaTiO_3$ glycolate powders can be controlled by varying the reaction conditions such as the reaction temperature and Ba:Ti molar ratio of starting precursors. After glycothermal treatment at $220^{\circ}C$ for 24 h in 1.25:1(Ba:Ti), the average particle size of the $BaTiO_3$ glycolate powder was about 200-400 nm and low agglomeration. $BaTiO_3$ powders were formed by heat-treating the glycolate powder in air at $500-1000^{\circ}C$. As a result, the size of $BaTiO_3$ crystallites changed from around 50-300 nm. It is also demonstrated that the size and shape of $BaTiO_3$ particles investigated as a function of calcination temperature. The $BaTiO_3$ particles obtained from optimum synthesis condition were pressed, sintered and measured for the dielectric property. The $BaTiO_3$ ceramics sintered at $1250^{\circ}C$ for 2 h had 98 % of theoretical density. The ceramics have an average grain size of about $1\;{\mu}m$ and displays the high dielectric constant (~3100) and low dielectric loss (<0.1) at room temperature.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.386-386
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• 2012

For white light emitting diode (LED) applications, it has been reported that Y3Al5O12:Ce3+ (YAG:Ce) in nano-sized phosphor performs better than it does in micro-sized particles. This is because nano-sized YAG:Ce can reduce internal light scattering when coated onto a blue LED surface. Recently, there have been many reports on the synthesis of nano-sized YAG particles using bottom-up method, such as co-precipitation method, sol-gel process, hydrothermal method, solvothermal method, and glycothermal method. However, there has been no report using top-down method. Top-down method has advantages than bottom-up method, such as large scale production and easy control of doping concentration and particle size. Therefore, in this study, nano-sized YAG:Ce phosphors were synthesized by a high energy beads milling process with varying beads size, milling time and milling steps. The beads milling process was performed by Laboratory Mill MINICER with ZrO2 beads. The phase identity and morphology of nano-sized YAG:Ce were characterized by X-ray powder diffraction (XRD) and field-emission scanning electron microscopy (FESEM), respectively. By controlling beads size, milling time and milling steps, we synthesized a size-tunable and uniform nano-sized YAG:Ce phosphors which average diameters were 100, 85 and 40 nm, respectively. After milling, there was no impurity and all of the peaks were in good agreement with YAG (JCPDS No. 33-0040). Luminescence and quantum efficiency (QE) of nano-sized YAG:Ce phosphors were measured by fluorescence spectrometer and QE measuring instrument, respectively. The synthesized YAG:Ce absorbed light efficiently in the visible region of 400-500 nm, and showed single broadband emission peaked at 550 nm with 50% of QE. As a result, by considering above results, high energy beads milling process could be a facile and reproducible synthesis method for nano-sized YAG:Ce phosphors.