• Bulletin of the Korean Chemical Society
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• v.25 no.5
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• pp.681-686
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• 2004

Ti-ZSM-5 prepared by secondary synthesis, from the reaction of H-ZSM-5 with vapor phase $TiCl_4$, was characterized with several physicochemical techniques including FT-IR and UV/VIS-DRS. It was found that zeolite structure, surface area and pore volume did not change, and the framework aluminum could not be replaced by titanium atom during the secondary synthesis of Ti-ZSM-5. The incorporation of titanium into the framework might be due to reaction of $TiCl_4$with the silanol groups associated with defects or surface sites. The formation of extra-framework titanium could not be avoided, unless the samples were further treated by water vapor at 550 $^{\circ}C$ or higher temperature. High temperature steam treatment of Ti-ZSM-5 prepared by chemical vapor deposition with $TiCl_4$was efficient to prevent the formation of non-framework titanium species. Ti-ZSM-5 zeolites prepared in this work contained only framework titanium species and exhibited improved catalytic property close to TS-1 prepared by hydrothermal synthesis.

• Journal of Powder Materials
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• v.23 no.4
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• pp.311-316
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• 2016

$Ni(OH)_2$ hollow spheres have been prepared by solvent displacement crystallization using a micro-injection device, and the effect of process parameters such as concentration and the relative ratio of the injection speed of the precursor solution, which is an aqueous solution of $NiSO_4{\cdot}6H_2O$, to isopropyl alcohol of displacement solvent have been investigated. The crystal phases after NaOH treatment are in the ${\beta}-phase$ for all process parameters. A higher concentration of $NiSO_4{\cdot}6H_2O$ aqueous solution is injected by a micro-injection device and bigger $Ni(OH)_2$ hollow spheres with a narrower particle size distribution are formed. The crystallinity and hardness of the as-obtained powder are so poor that hydrothermal treatment of the as-obtained $Ni(OH)_2$ at $120^{\circ}C$ for 24 h in distilled water is performed in order to greatly improve the crystallinity. It is thought that a relative ratio of the injection speed of $NiSO_4{\cdot}6H_2O$ to that of isopropyl alcohol of at least more than 1 is preferable to synthesize Ni(OH)2 hollow spheres. It is confirmed that this solution-based process is very effective in synthesizing ceramic hollow spheres by simple adjustment of the process parameters such as the concentration and the injection speed.

• Journal of Powder Materials
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• v.15 no.2
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• pp.125-135
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• 2008

[ $TiO_2$ ] nanotubes for photocatalytic application have been synthesized by hydrothermal method. $TiO_2$ nanotubes are formed by washing process after reaction in alkalic solution. Nanotubes with different morphology have been fabricated by changing NaOH concentration, temperature and time. $TiO_2$ nanoparticles were treated inside NaOH aqueous solution in a Teflon vessel at $110^{\circ}C$ for 20 h, after which they were washed with HCl aqueous solution and deionized water. Nanotube with the most perfect morphology was formed from 0.1 N HCl washing treatment. $TiO_2$ nanotube was also obtained when the precursor was washed with other washing solutions such as $NH_4OH$, NaCl, $K_2SO_4$, and $Na_2SO_3$. Therefore, it was suggested that $Na^+$ ion combined inside the precursor compound slowly comes out from the structure, leaving nanosheet morphology of $TiO_2$ compounds, which in turn become the nanotube in the presence of hydroxyl ion. To stabilize the sheet morphology, the different type of washing treatment solution might be considered such as amine class compounds.

• Journal of the Korean Ceramic Society
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• v.39 no.3
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• pp.245-251
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• 2002

We prepared γ-alumina beads using the amorphous alumina, obtained by fast calcination of gibbsite, and its were immersed in aqueous solution of the mixture of 21.87% nitric acid and 28.57% acetic acid. The beads thus were hydrothermaly treated at 200$^{\circ}$C for 3h, and were investigated changes of crystal, pore characteristics, $N_2$ adsorption and desorption isotherms, mechanical strengths and thermal resistance. Acicular platelet crystals of 0.1∼0.3${\mu}$m were transformed into acicular boehmite crystals of 1∼2${\mu}$m having the same crystal structure. Through this changes, we found that reversible phase transformation due to hydrothermal reaction took placed between boehmite and ${\gamma}$-alumina. In comparison to the ${\gamma}$-alumina bead before hydrothermal treatment, $N_2$ adsorption capacity was increased from 450㎖/g to 670㎖/g, and pore volume between 100${\AA}$ and 1000${\AA}$ was increased form 0.15㎖/g to 0.77㎖g, and mechanical strength was increased form 1.4MPa to 2.2MPa. Also, it showed the remarkable thermal resistance which sustained ${\theta}$-alumina crystal structure and pores between 100${\AA}$ and 1000${\AA}$ at 1000$^{\circ}$C in 40vol% steam.

• Ocean and Polar Research
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• v.36 no.4
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• pp.383-394
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• 2014

The surface sediments from the manganese nodule exploration area of Korea in the Clarion-Clipperton fracture zone were investigated to understand the resource potential of and emplacement mechanism for rare earth elements (REEs). The sediments are categorized into three lithological units (Unit I, II and III from top to bottom), but into two groups (Unit I/II and Unit III) based on the distribution pattern of REEs. The distribution pattern of REEs in Unit I/II is similar to that of Post-Archean Australian Shale (PAAS), but shows a negative Ce anomaly and enrichment in heavy REEs (HREEs). In Unit III, the HREE enrichment and Ce anomaly is much more remarkable than Unit I/II when normalized to PAAS, which are interpreted as resulting from the absorption of REEs from seawater by Fe oxyhydroxides that were transported along the buoyant plume from remotely-located hydrothermal vents. It is supported by the PAAS-normalized REE pattern of Unit III which is similar to those of seawater and East Pacific Rise sediments. Meanwhile, the PAAS-normalized REE pattern of Unit I/II is explained by the 4:1 mixing of terrestrial eolian sediment and Unit III from each, indicating the much smaller contribution of hydrothermal origin material to Unit I/II. The studied sediments have the potentiality of a low-grade and large tonnage REE resource. However, the mining of REE-bearing sediment needs a large size extra collecting, lifting and treatment system to dress and refine low-grade sediments if the sediment is exploited with manganese nodules. It is economically infeasible to develop low-grade REE sediments at this moment in time because the exploitation of REE-bearing sediments with manganese nodules increase the mining cost.

• 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.50 no.1
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• pp.25-29
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• 2012

$TiO_2$ nanotubes are prepared from rutile prticles via an alkaline hydrothermal synthesis and the consequent heat treatment at $300{\sim}500^{\circ}C$. The physical and electrochemical properties of the $TiO_2$ nanotubes are characterized for use as a anode material of rechargeable lithium battery. In particular, the microscale dusts as an impurity component occurred in the purification step after the hydrothermal reaction are completely removed to yield $TiO_2$ nanotube with a higher specific surface area and more obvious crystalline phases. As the annealing temperature increases, the specific surface area is slightly decreased due to some aggregation between the isotropically dispersed nanotubes. Highest initial discharge capacity of 250 mAh $g^{-1}$ is achieved for the $TiO_2$ nanotube annealed at $300^{\circ}C$, whereas the $400^{\circ}C$ $TiO_2$ nanotube shows the superior cycle performance and high-rate capability.

• Journal of the Mineralogical Society of Korea
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• v.20 no.2 s.52
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• pp.71-81
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• 2007

The marble-type dolomite from the Jasung Mine, which was farmed by duplicated affects of contact metamorphism and subsequent hydrothermal alteration, corresponds to a high-purity dolomite ranging up to above 98wt.% in dolomite contents. The dolomite contain minor impurities such as quartz, muscovite, and pyrite. It is characteristic that the dolomite is fairy Fe-rich corresponding to 0.4 wt.% due to the presence of pyrite of possible hydrothermal origin. The dolomite is nearly white-colored and constituting with subhedral crystals ranging $0.35{\sim}0.46mm$M in size, forming equigranular texture. Compared to the typical high-Ca limestone from the Pungchon Formation, the powder characteristics of dolomite is rather superior in milling efficiency, yields of fine particles, and size distribution. In addition, except for iron contents, the dolomite powder is no less superior than the limestone in quality and characteristics as fillers with respects to not only whiteness, oil absorption, and specific surface area but also shape characters such as elongation ratio, aspect ratio, and sphericity. This good characteristics of dolomite powder seem to be originated basically from comparatively higher grade and crystallinity of dolomite. Higher iron contents and the presence of sulfides prevents the dolomite from application for uses by thermal treatment, except for metallic manufacture. However, if proper ore separation procedure is available, the dolomite can be sufficiently utilized as substitutes for high-Ca limestone in most fields of filler industries.

• Journal of the Korean Electrochemical Society
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• v.16 no.3
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• pp.151-156
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• 2013

As the cathode material for li-ion battery, $LiNi_{0.5}Mn_{0.3}Co_{0.2}O_2$ were synthesized by supercritical hydrothermal method and calcined $850^{\circ}C$ and $900^{\circ}C$ for 10hrs in air. The effect of temperature in the heat treatment on the powder and its performance were studied of xray diffraction pattern, SEM-image, physical properties and electrochemical behaviors. As a result, calcined at $900^{\circ}C$ material particle size more increase than calcined at $850^{\circ}C$ material, especially shows excellent electrochemical performance with initial reversible specific capacity of 163.84 mAh/g (0.1C/2.0-4.3V), 186.87 mAh/g (0.1C/2.0-4.5V) and good capacity retention of 91.49% (0.2C/2.0-4.3V) and 90.36% (0.2C/2.0-4.5V) after 50th charge/discharge cycle.

• Applied Chemistry for Engineering
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• v.26 no.2
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• pp.217-223
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• 2015

Effects of the post-acid treatment of SAPO-34 sample by hydrochloric acid were investigated to enhance the catalytic performance in DTO reaction. Uniformly sized SAPO-34 samples with cubic-like morphology were prepared by hydrothermal method using TEAOH and DEA as the structure directing agents. It was modified in terms of the HCl concentration and treating time. As a result, the total surface area and micropore volume for the well modified samples increased and the total acid site was somewhat decreased along with the erosion of the external surface. Especially, the catalytic lifetime and light olefins selectivity for acid treated SAPO-0.2 M (3 h) samples were considerably enhanced compared with those of untreated SAPO-34 samples. It indicates that the deactivation by coke formation proceeds mainly at the pore entrance on the external surface. Therefore, the acid treatment was confirmed to be a simple method which can significantly improve the catalytic performance by modifying the external surface of SAPO-34 catalyst.