• Journal of Magnetics
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• v.15 no.4
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• pp.179-184
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• 2010

We have investigated the effects of post annealing on iron oxide nanoparticles synthesized by the novel hydrothermal synthesis method with the $FeSO_4{\cdot}7H_2O$. To investigate the post annealing effect, the as-synthesized iron oxide nanoparticles were annealed at different temperatures in a vacuum chamber. The morphological, structural and magnetic properties of the iron oxide nanoparticles were investigated with high resolution X-ray powder diffraction (XRD), high resolution transmission electron microscopy (HRTEM), Mossbauer spectroscopy, and vibrating sample magnetometer analysis. According to the XRD and HRTEM analysis results, as-synthesized iron oxide nanoparticles were only magnetite ($Fe_3O_4$) phase with face-centered cubic structure but post annealed iron oxide nanoparticles at $700^{\circ}C$ were mainly magnetite phase with trivial maghemite ($\gamma-Fe_2O_3$) phase which was induced in the post annealing treatment. The crystallinity of the iron oxide nanoparticles is enhanced by the post annealing treatment. The particle size of the as-synthesized iron oxide nanoparticles was about 5 nm and the particle shape was almost spherical. But the particle size of the post annealed iron oxide nanoparticles at $700^{\circ}C$ was around 25 nm and the particle shape was spherical and irregular. The as-synthesized iron oxide nanoparticles showed superparamagnetic behavior, but post annealed iron oxide nanoparticles at $700^{\circ}C$ did not show superparamagnetic behavior due to the increase of particle size by post annealing treatment. The saturation of magnetization of the as-synthesized nanoparticles, post annealed nanoparticles at $500^{\circ}C$, and post annealed nanoparticles at $700^{\circ}C$ was found to be 3.7 emu/g, 6.1 emu/g, and 7.5 emu/g, respectively. The much smaller saturation magnetization value than one of bulk magnetite can be attributed to spin disorder and/or spin canting, spin pinning at the nanoparticle surface.

• Resources Recycling
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• v.28 no.6
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• pp.46-53
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• 2019

Cement mortar was hydrothermal-synthesized with particle size of tailings using scheelite tailings deposited without proper treatment, and its physical properties were investigated. The mixing ratios of water-cement and sand-cement were fixed at 75 % and 400 %, respectively, during preparing cemnt mortar, and the sand was replaced by the tailings at 0 ~ 50 %. The particle size of tailings was controlled at 9.3 ~ 53.0 ℃, and the hydrothermal temperature was kept at 60 ~ 180 ℃ for 6 hours after the temperature increased to pretermined temperature with 2 ℃ heating rate. The compressive strength increased with increasing hydrothermal temperature. The compressive strengths were 55.2 MPa and 54.5 MPa when the mortars were prepared with 30 % low arsenic and high arsenic tailings after 60 min grinding. The compresiive strenght was enhanced 300 % compared with reference sample.

• Korean Journal of Materials Research
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• v.14 no.9
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• pp.607-613
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• 2004

This study was to investigate the surface properties of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Anodizing was performed at current density 30 $mA/cm^2$ up to 300 V in electrolyte solutions containing $DL-{\alpha}$-glycerophosphate disodium salt hydrate($DL-{\alpha}$-GP) and calcium acetate (CA). Hydrothermal treatment was done at $300^{\circ}C$ for 2 hrs to produce a thin outermost layer of hydroxyapatite (HA). The bioactivity was evaluated from HA formation on the surfaces in a Hanks' solution with pH 7.4 at $36.5^{\circ}C$ for 30 days. The size of micropores and the thickness of oxide film increased and complicated multilayer by increasing the spark forming voltage. Needle-like HA crystals were observed on anodic oxide film after the hydrothermal treatment at $300^{\circ}C$ for 2 hrs. When increasing $DL-{\alpha}$-GP in electrolyte composition, the precipitated HA crystals showed the shape of thick and shorter rod. However, when increasing CA, the more fine needle shape HA crystals were appeared. The bioactivity in Hanks' solution was accelerated when the oxide films composed with strong anatase peak with presence of rutile peak. The increase of amount of Ca and P was observed in groups having bioactivity in Hanks' solution. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal and it was closer to 1.67 as increasing the immersion time in Hanks' solution.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.7 no.3
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• pp.437-448
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• 1997

The substitution of vanadium atoms into the zeolite framework structure could be applied to the large pore zeolites by means of modified treatments as well as direct hydrothermal synthesis. The incorporation of V into the zeolite framework was demonstrated by instrumental analysis techniques. The result of X-ray diffraction analysis showed that the unit cell parameters increased after incorporation of vanadium into the zeolitic lattice, indicating that the replacement of Si by the larger V atoms could cause a slight expansion in the unit cell. In addition, the results of FTIR, Uv-Vis and Si-MAS-NMR spectra strongly support the incorporation of V into the zeolite framework. Acid leaching of aluminum in zeolites can provide a vacant position in the lattice for the insertion of vansdium by secondary hydrothermal treatment.

• Journal of Environmental Science International
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• v.12 no.12
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• pp.1321-1327
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• 2003

Two different kinds of cases, with and without addition of noncrystalline silica to the Hadong kaolin were studied to obtain useful information on the synthesis of zeolite. The research was carried out to investigate the formation area and the crystalized degree of zeolite according to a synthetic time, the water content of raw material mixture, KOH concentration, and stirring intensity. In the case of without addition of noncrystalline silica to the Hadong kaolin and the low concentration range of KOH, the structure of the kaolin was not changed. However, when the mole ratio of K2O/SiO$_2$ in natural kaolin was increased, Linde-L zeolite and unknown structure of kaolins, U-1 and U-2 were produced. While in the high concentration range of KOH, the unknown structure of kaolins, U-6 and U-2, were produced and the production rate of U-6 was increased with the increased of K2O/SiO$_2$ mole ratio. In the case of with addition of noncrystalline silica to the Hadong kaolin and treatment with KOH hydrothermal processing, ZSM-5, ZSM-35, and Linde-L zeolites and the mixture of unknown structure of zeolites, U-1, U-2, U-3, and U-4, were obtained. Both cases demonstrated that the synthesis of zeolite from the Hadong kaolin was highly influenced by KOH concentration of raw material mixture.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.8 no.4
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• pp.563-566
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• 1998

$BaTiO_3$ fine particles were prepared by hydrothermal process from titanium tetra-isoproproxide ($Ti(OiPr)_4$) and barium hexa-hydroxide ($Ba(OH)_2{cdot}8H_2O$) as raw materials. The fine particles were obtained at the temperature range of 160 to $185^{\circ}C$. The properties of $BaTiO_3$ particles were studied as a function of various parameters such as reaction temperature, reaction time and Ba/Ti ratio, etc. The average particle size of $BaTiO_3$ increased with increasing reaction temperature and time. After hydrothermal treatment at $170^{\circ}C$ for 8 h, the average particle size of $BaTiO_3$ was about 30 nm and the particle size distribution was narrow.

• Journal of the Korean Ceramic Society
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• v.32 no.7
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• pp.777-782
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• 1995

The scale up production test for the hydrothermal synthesis of clay mineral from the anorthite, which is distributed in San Chung-District of Korea and called as the ground rock for halloysite-kaolin, has been investigated by using the gaitator type reactor. The automatic control system has been developed and applied for the more effective producibility and the reduction in the defect of this intermittent batch processing property, and finally for the feasibility of this system in actual use. It was observed that this agitator type reactor can reduce the synthesis reaction tme from 5 days to 3 days, only with the condition of 20rpm. The automatic control system could regulate the vessel temperature and pressure precisely at an optimum condition during the treatment. Therefore, from these test results the application-possibility for this system was found to be feasible in actual use.

• Journal of Environmental Science International
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• v.22 no.7
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• pp.837-845
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• 2013

This study was designed to synthesize mesoporous carbon, porous carbonic material and to characterize its surface in an attempt to adsorption methane gas($CH_4$). Synthesis of mesoporous carbon was carried out under two steps ; 1. forming a RF-silica complex with a mold using CTMABr, a surfactant, and TEOS, raw material of silica, and 2. eliminating silica through carbonization and HF treatment. The mesoporous carbon was synthesized under various conditions of synthesis time and calcination. Eight different types of mesoporous carbon, which were designated as MC1, MC2, MC3, MC4, MCT1, MCT2, MCT3, and MCT4, were prepared depending upon preparation conditions. The analysis of mesoporous carbon characteristics showed that the calcination of silica stabilized the mixed structure of silica and carbonic complex, and made the particle uniform. The results also showed that hydrothermal synthesis time did not have a strong influence on the size of pore. The bigger specific surface area was obtained as the hydrothermal synthesis time was extended. However, the specific surface area was getting smaller again after a certain period of time. In adsorption experiments, $CH_4$ was used as adsorbate. For the case of $CH_4$, MCT3 showed the highest adsorption efficiency.

• Bulletin of the Korean Chemical Society
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• v.25 no.9
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• pp.1341-1345
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• 2004

We developed a novel synthesis strategy of titania nanowire arrays by employing simple hydrothermal reaction and ion-exchange reaction techniques. Hydrothermal reactions of metallic titanium powder with $H_2O_2$ in a 10 M NaOH solution produced a new sodium titanate compound, $Na_2Ti_6O_{13}{\cdot}xH_2O$ (x~4.2), as arrays of nanowires of lengths up to 1 mm. Acid-treatment followed by calcination of this material produced arrays of highly crystalline anatase nanowires as evidenced by x-ray diffraction, Raman spectroscopy, and transmission electron microscopy studies. In both cases of sodium titanate and anatase, the nanowires have exceptionally large aspect ratios of 10,000 or higher, and they form arrays over a large area of $1.5 {\times} 3 cm^2$. Observations on the reaction products with varied conditions indicate that the array formation requires simultaneously controlled formation and crystal growth rates of the $Na_2Ti_6O_{13}{\cdot}xH_2O$ phase.

• Korean Journal of Environmental Agriculture
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• v.24 no.3
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• pp.232-237
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• 2005

This study was conducted to elucidate the effects of NaOH fusion treatment on Na-P1 zeolite synthesis from fly ash and to evaluate its optimal condition. NaOH fusion treatment of fly ash led to Na-P1 zeolite with shorter reaction time and higher quality compared that of simple hydrothermal method. Mixed zeolite phases of Na-P1 and hydroxy sodalite were formed by the fusion treatment below $450^{\circ}C$, whereas only Na-P1 zeolite was formed above $550^{\circ}C$. Ratio of NaOH/fly ash, reaction times, fusion temperature and solid/liquid ratio strongly affected the kind and crystallinity of the zeolite formed. The CEC of Na-P1 zeolite formed at the optimum reaction conditions of NaOH/fly ash ratio 0.9 and solid/liquid ratio $1/5.0{\sim}1/7.5$ after NaOH fusion treatment at $550^{\circ}C$ for 2 hours was about $398cmol^+kg^{-1}$ which was 40% higher than those of control products. Therefore, it is clear that NaOH fusion treatment of fly ash in open system could lead to Na-P1 zeolite with high purity.