• Applied Chemistry for Engineering
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• v.28 no.6
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• pp.705-713
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• 2017

A novel material, $Bi_2WO_6-GO-TiO_2$ composite, was successfully synthesized using a facile hydrothermal method. During the hydrothermal reaction, the loading of $Bi_2WO_6$ and $TiO_2$ nanoparticles onto graphene sheets was achieved. The obtained $Bi_2WO_{6-GO-TiO2}$ composite photo-catalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM), Raman spectroscopy, ultraviolet-visible diffuse reflectance spectroscopy (UV-vis-DRS), and X-ray photoelectron spectroscopy (XPS). The $Bi_2WO_6$ nanoparticle showed an irregular dark-square block nanoplate shape, while $TiO_2$ nanoparticles covered the surface of the graphene sheets with a quantum dot size. The degradation of rhodamine B (RhB), methylene blue trihydrate (MB), and reactive black B (RBB) dyes in an aqueous solution with different initial amount of catalysts was observed by UV spectrophotometry after measuring the decrease in the concentration. As a result, the $Bi_2WO_6-GO-TiO_2$ composite showed good decolorization activity with MB solution under visible light. The $Bi_2WO_6-GO-TiO_2$ composite is expected to become a new potential material for decolorization activity. Photocatalytic reactions with different photocatalysts were explained by the Langmuir-Hinshelwood model and a band theory.

• Applied Chemistry for Engineering
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• v.9 no.5
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• pp.654-660
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• 1998

In preparing PSZT powder by hydrothermal synthesis, effects of reaction temperature, concentration of raw materials and mineralizer on crystallinity, particle size distribution, and dielectric constant were investigated. By varying the concentration of mineralizer and the ratio of Pb to Sr or Zr to Ti, crystalline PSZT powder, having the mean particle size of $0.3{\sim}15{\mu}m$, was prepared by hydrothermal synthesis in the temperature range of $120{\sim}200^{\circ}C$ for a 2h reaction. PSZT ceramics, having dielectric constant of 1000~3000, were prepared at $1150^{\circ}C$ for a 2h sintering reaction of the PSZT powders. Experimental results showed that the weight mean particle size of $0.5{\mu}m$ was obtained when the concentration of KOH in the solution was 10 wt % and the ratio of Pb to Sr was 0.95/0.05, that of Zr to Ti was 0.52/0.48. It also showed that the ceramics of dielectric constant of 2900 were prepared through sintering of this PSZT powder. Size of PSZT particles became smaller with its narrow distribution as the concentration of KOH increased up to 10 wt %. However, it came to be larger at this concentration and above. By adding small amount of Sr that would not affect that crystallinity of particles we can improve dielectric property of sintered materials. Addition of Zr may shift the major crystal phase of synthetic PSZT powder from tetragonal to rhombohedral phase.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.5
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• pp.203-207
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• 2019

Calcium phosphates such as hydroxyapatite (HAp), tricalcium phosphate (${\beta}$-TCP), and biphasic calcium phosphate (BCP, HAp/${\beta}$-TCP) have been prepared via hydrothermal treatment. The synthesis was conducted by reacting ($Ca(OH)_2$) aqueous solution with phosphoric acid ($H_3PO_4$) under different hydrothermal synthesis conditions (temperatures up to $150^{\circ}C$ and pH lower than 12). The effects of initial precursor Ca/P ratio (1.30, 1.50 and 1.67) and post heat treatment on the phase evolution behavior of the powders and sintered ceramics were investigated. The phases of resulting powders and sintered ceramics were controllable by adjusting the initial Ca/P ratio. A single HAp phase without any noticeable second phase was obtained for the initial Ca/P ratio of 1.67 in the overall heat treatment range. Pure ${\beta}$-TCP and biphasic calcium phosphate (HAp/${\beta}$-TCP) were synthesized from precursor solutions having Ca/P molar ratios of 1.30 and 1.50, respectively, after having been heat treated at $900^{\circ}C$ or higher. Dense ceramics with translucency were obtained at considerably lower sintering temperatures.

• Journal of the Korea Organic Resources Recycling Association
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• v.31 no.3
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• pp.15-25
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• 2023

In this study, silicon sludge from semiconductor dicing process is recycled to fabricate silica nanoparticles, which are applied as dispersing materials for electro-responsive (ER) smart fluid. In specific, metal impurities are removed from silicon sludge by acid washing to obtain the high-purity silicon powder. And then, silica nanoparticles are synthesized by facile hydrothermal method employing the silicon powder as reactant material. To control the size of silica nanoparticles, the reaction time of hydrothermal method is varied as 8, 15, 20, and 30 hours are applied to control the size of silica nanoparticles. Sizes of silica nanoparticles are increased proportionally to the reaction time owing to the increased numbers of hydrolysis and condensation reactions. As-synthesized silica nanoparticles are prepared as electro-responsive smart fluids by dispersing into silicon oil. Silica nanoparticles synthesized by 30 hours of hydrothermal reaction (SiO₂-H30) exhibit the highest shear stress of 21.4 Pa under an applied electric field strength of 3.0kV mm^-1. Such enhancement in ER performance of SiO₂-H30 among various silica nanoparticles are attribute to the reinforcing effect originated from the mixed particle size, which allowing the formation of rigid chain-like structures. Accordingly, this study successfully propose a recycling method of silicon sludge to synthesize silica nanoparticles and their derived ER fluids, which may suggest new possibility to ESG management emphasizing the eco-friendliness.

• Journal of the Mineralogical Society of Korea
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• v.20 no.1 s.51
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• pp.1-6
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• 2007

Hectorite was synthesized by a two-step hydrothermal process from $Mg(OH)_{2}$, water glass (${\sim}30\;wt%\;SiO_{2}$) and Li-compound at $90{\pm}5^{\circ}C$. The product shows excellent dispersion and swelling properties. The mixture of the starting materials was heated in a glass vessel for the first reaction with continuous stirring and the pH of the solution was adjusted to $6{\sim}8$, resulting in the formation of a precursor of hectorite. The excess salt components were washed out from the resulting slurry and then was matured in the glass vessel for the 2nd reaction. Li compound was added during the reaction. After a 10 h retention, the gel of hectorite was formed. The XRD pattern of the synthesized one was coincided with that of natural hectorite and SEM study revealed uniform grains 50 m in diameter. The d001 basal spacing of the product moved from 12 to $17.4\;{\AA}$ after glycolation treatment. The measured value of CEC and the swelling capacity was 90 cmol/kg and $60{\sim}70\;mL/2\;g$, respectively.

• Korean Chemical Engineering Research
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• v.57 no.1
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• pp.133-141
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• 2019

High specific surface area zirconia with acid-basic property was synthesized by precipitation using reflux method or hydrothermal synthesis method using ammonium hydroxide solution as precipitant in the range of pH of Zr solution from 2 to 10. The prepared zirconia was characterized by the nitrogen adsorption, X-ray diffraction (XRD), isopropanol temperature programmed desorption (IPA-TPD), scanning electron microscopy and X-ray photoelectron spectroscopy, and the catalytic activity in the IPA decomposition reaction was correlated with the acid-basic properties. When using reflux method, high pH of Zr solution was required to obtain high fraction of tetragonal zirconia, and pure tetragonal zirconia was possible at pH 9 or higher. High pH was required to obtain high specific surface area zirconia, and the hydrous zirconia synthesized at pH 10 had high specific surface area zirconia of $260m^2g^{-1}$ even after calcination at $600^{\circ}C$. However, hydrothermal synthesis with high pressure under the same conditions resulted in very low specific surface area below $40m^2g^{-1}$ and monoclinic phase zirconia was synthesized. High pH of the solution was required to obtain high specific surface area tetragonal phase zirconia. In hydrothermal synthesis requiring high pressure, monoclinic zirconia was produced irrespective of the pH of the solution, and the specific surface area was relatively low. Zirconia with high specific surface area and tetragonal phase was predominantly acidic compared to basicity and only propylene, which was observed as selective dehydration reaction in IPA decomposition reaction, was produced.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.269-269
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• 2012

수산화인회석(Hydroxyapatite)는 뼈와 이빨의 무기물 주성분으로서, 칼슘과 인산염으로 구성된다. 우리는 수산화인회석의 합성에 용융열 합성법(molten salt method), 수열 합성법(hydrothermal method), 용매열 합성법(solvothermal method)을 사용하였으며, pH 조절과 각기 다른 용매를 사용하여 다양한 형태의 수산화인회석을 합성하였다. TEM과 SEM을 이용하여 크기와 모양이 제어된 수산화인회석임을 확인할 수 있었다. 합성된 수산화인회석을 이용하여, 전이금속 Ruthenium cation을 Hydroxyapatite 표면에 ion-exchange 반응을 통하여 도입하였으며, ICP를 통하여 Ru 함양을 정량하였다. 합성된 Ruthenium Hydroxyapatite (Ru-HAP)를 이용하여 dimethylamine borane를 통한 수소 발생을 확인하였다.

• Clean Technology
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• v.26 no.4
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• pp.263-269
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• 2020

Zeolite was synthesized hydrothermally using the water-treatment sludge, and the effects of various synthesis parameters like reaction temperature, reaction time, and Na2O/SiO2 molar ratio on the crystallization of zeolite were investigated. Crystal structure, physical property, and thermal stability of zeolite crystals were characterized by X-ray powder diffraction, FTIR spectroscopy, BET nitrogen adsorption, and TGA measurements. The removal efficiencies of nitrogen in ammonia, heavy metal ions, and TOC were calculated to evaluate zeolite's adsorption capacity. The primary chemical composition of water-treatment sludge was 28.79% Al2O3 and 27.06% SiO2. The zeolites were synthesized by merely employing the water-treatment sludge as silica and alumina sources without additional chemicals. Zeolite crystals synthesized through the water-treatment sludge were confirmed as an A-type zeolite structure. Zeolite A had the highest crystallinity obtained from a gel with the molar composition 2.1Na2O-Al2O3-1.6SiO2-65H2O after 5 h at a temperature of 90 ℃. The specific surface area of zeolite obtained was 55 ㎡ g-1, which was higher than commercial zeolite A. The removal efficiency of nitrogen in ammonia was 68% after 3 h of reaction time, while the removal efficiencies of Pb2+ and Cd2+ ions were 99.1% and 99.3%, respectively. These results indicate active ion exchange between Pb2+ or Cd2+ ion and Na+ ion in the zeolite framework. The adsorption experiments on the different zeolite addition conditions were performed for 3 h with 300 ppm humic acid. Based on the results, TOC's highest efficiency was 83% when 5 g of zeolite was added.

• 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 the Korean Chemical Society
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• v.45 no.6
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• pp.507-512
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• 2001

The hydrothermal reaction between lanthanum(Ⅲ) nitrate $(La(NO3)3${\cdot}$6H_2O)$ and benzene-1,3-dicarboxylic acid $(H_2BDC)$ in the presence of 1,2-bis(4-pyridyl)ethane gave a 2-D lanthnum-BDC coordination polymer with an empirical formula of $〔La_4$(BDC)_6(H_2O)_5$〕(H_2O)$ (1). X-ray structure analysis of compound 1 revealed that this polymer contains four distinct La metals. The three La metals are 7-coordinate with three different structures: a capped trigonal prism, a capped octahedron, and a pentagonal bipyramid. The remaining La metal has a 8-coordinate, square antiprismatic structure.