• 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.34 no.11
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• pp.1159-1164
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• 1997

Magnetite(Fe3O4) powders were synthesized through glycothermal reaction by using crystalline $\alpha$-FeOOH as precursor and ethyleanne glycol as solvent. The phase, morphology and particle size of synthesized powders were characterized by XRD and an SEM. When only ethylene glycol was used as solvent, the phase was transformed from $\alpha$-FeOOH to $\alpha$-Fe2O3 and finally Fe3O4 at 27$0^{\circ}C$ for 6hr without morphological change. But by addition of water, Fe3O4 powders were synthesized at 23$0^{\circ}C$ for 3hr through solution-recrystalization process. As the content of water addition increased, the particle shape changed from sphere to octahedron and the partcle size increased. When the excess amount of water added, residual $\alpha$-FeOOH or $\alpha$-Fe2O3 was recrystalized.

• 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 Korea Association of Crystal Growth Conference
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• 1996.06a
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• pp.497-501
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• 1996

The ZnFe2O4 powder were prepared under glycothermal conditions by precipitation from metal nitrates with aqueous potassium hydroxide. Ultrafine particles of the ZnFe2O4 were obtained at temperatures as low as 225-300$^{\circ}C$. The microstructure and phase of the ZnFe2O4 powder was studied by SEM and XRD. The properties of the powder were studied as a function of various parameters (reaction temperature, reaction time, solid loading). The average particle diameter of the ZnFe2O4 increased with increasing reaction temperature. After glycothermal treatment at 270$^{\circ}C$ for 8hrs., the average particle diameter of the ZnFe2O4 was about 50 nm.

• 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 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.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.7 no.1
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• pp.167-173
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• 1997

The $ZnFe_2O_4$ powder was prepared under glycothermal conditions by precipitation from metal nitrates with aqueous potassium hydroxide. The fine powder was obtained at temperatures as low as 225 to $300^{\circ}C$. The microstructure and phase of the $ZnFe_2O_4$ powder were studied by SEM and XRD. The properties of the powder were studied as a function of various parameters (reaction temperature, reaction time, solid loading, etc). The average particle size of the $ZnFe_2O_4$ increased with increasing reaction temperature. After glycothermal treatment at $270^{\circ}C$ for 8 h, the average particle diameter of the $ZnFe_2O_4$ was about 50 nm.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.7 no.4
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• pp.567-572
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• 1997

The ZnO powder was prepared under glycothermal conditions by precipitation from metal nitrates with aqueous potassium hydroxide. The fine powder was obtained at temperatures as low as 225 to $275^{\circ}C$, The microstructure and phase of the powder were studied by SEM and XRD. The properties of the ZnO powder were studied as a function of various parameters (reaction temperature, reaction time, solid loading, etc). The average particle size of the ZnO increased with increasing reaction temperature. After glycothermal treatment at $225^{\circ}C$ for 8 h, the average particle size of the ZnO powder was about 150 nm and the particle size distribution was narrow.