• 한국재료학회지
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• 제19권8호
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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.

• 한국세라믹학회지
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• 제39권7호
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• pp.642-648
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• 2002

본 연구에서는 TiCl$_4$를 가수분해 시켜 제조한 비정질의 titanium hydrous gel과 Ba(OH)$_2$.8$H_2O$를 출발물질로 사용하였으며, 반응용매로써 1,4-butanediol과 distilled water를 이용하여 나노 사이즈 BaTiO$_3$분말을 제조하였다. 용매로써 사용된 1,4-butanediol과 distilled water의 부피비에 따라 입자의 크기를 조절할 수 있으며, 습식화학법의 단점이었던 분말의 응집을 최소화 시킬 수 있다. 그리고 22$0^{\circ}C$의 비교적 낮은 반응온도에서 분산성이 우수하고, 입도분포가 좁은 약 50~200nm의 barium titanate 나노 분말을 제조하였다.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2009년도 하계학술대회 논문집
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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.

• 한국세라믹학회:학술대회논문집
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• 한국세라믹학회 2003년도 추계총회 및 연구발표회 초록집
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• pp.169.2-169
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• 2003

• 한국재료학회지
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• 제27권9호
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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.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2006년도 하계학술대회 논문집 Vol.7
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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.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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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.