• Resources Recycling
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• v.31 no.1
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• pp.29-36
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• 2022

The hydrogen reduction behavior of molybdenum oxides was studied using a horizontal-tube reactor. Reduction was carried out in two stages: MoO₃ → MoO₂ and MoO₂ → Mo. In the first stage, a mixed gas composed of 30 vol% H₂ and 70 vol% Ar was selected for the MoO₃ reduction because of its highly exothermic reaction. The temperature ranged from 550 to 600 ℃, and the residence time ranged from 30 to 150 min. In the second step, pure H₂ gas was used for the MoO₂ reduction, and the temperature and residence time ranges were 700-750 ℃ and 30-150 min, respectively. The hydrogen reduction behavior of molybdenum oxides was found to be somewhat different between the two stages. For the first stage, a temperature dependence of the reaction rate was observed, and the best curve fittings were obtained with a surface reaction control mechanism, despite the presence of intermediate oxides under the conditions of this study. Based on this mechanism, the activation energy and pre-exponential were calculated as 85.0 kJ/mol and 9.18 × 10⁷, respectively. In addition, the pore size within a particle increases with the temperature and residence time. In the second stage, a temperature dependence of the reaction rate was also observed; however, the surface reaction control mechanism fit only the early part, which can be ascribed to the degradation of the oxide crystals by a volume change as the MoO₂ → Mo phase transformation proceeded in the later part.

• Korean Chemical Engineering Research
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• v.43 no.4
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• pp.503-510
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• 2005

In this research, composite alumina was prepared to add the various promoters by sol-gel method and examined its thermal stability. After sintering at $1,200^{\circ}C$, the thermal stability resulted in following order, $Si{\fallingdotseq}La$ > Ti > $Ba{\fallingdotseq}Ce$ > Y > $Zr{\fallingdotseq}Mg$, in accordance with adding the promoters. Especially in case of silica-added alumina, a phase transformation temperature to ${\alpha}$-alumina increased about $150^{\circ}C$ and after sintering at $1,200^{\circ}C$, it showed to maintain in ${\gamma}$-form and ${\delta}$-form alumina phase. Also it showed an increase of surface area from $3m^2/g$ to $71m^2/g$ compared with pure ${\alpha}$-alumina. In the case of silicaadded alumina, the characterization change of this alumina particle resulted in a delay of phase transformation because Si-O-Al bond was increased when sintered at high temperature. In case of lanthanum-added alumina, there was a sintering delay phenomenon in inter-particles as $LaAlO_3$ structure existed. The existence of lanthanum structure was confirmed by XRD and XPS analysis. It appeared on the alumina surface as $La_2O_3$ structure when it was sintered under $1,000^{\circ}C$, as the perovskite structure of $LaAlO_3$ at above $1,000^{\circ}C$ and as the magneto-plumbite structure of $LaAl_{11}O_{18}$ at above $1,300^{\circ}C$.

• Journal of the Mineralogical Society of Korea
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• v.24 no.2
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• pp.101-110
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• 2011

Charcoal burning in the process of manufacture and ordinary use often release many constituent chemical species. As a result of open burning, the chemical composition as well as the physical properties of original material changes through the modification of surface properties of charcoal. Surface modification could be more responsible toward the outside elements for surface adsorption, it becomes easy to adsorb more toxic elements through surface adsorption. In this study, four kinds of commercially available charcoal were studied against the chemical and thermal stability along with the heavy metals and organic hazardous substances. Thermo gravimetric analysis (TGA) and differential scanning calorimetry, from room temperature to $400^{\circ}C$, were performed to study the weight loss and the changes in the behavior of those substances. According to TGA analysis, about 10% of weight loss was happened before $200^{\circ}C$. It was found that related weight loss of this temperature region may responsible to the gas phase organic matter. Natural charcoal, K1 and C1 show 15% of loss during the reaction heated to $400^{\circ}C$, while the artificial charcoal K2, C2 show the weight loss of about 20% was found. This is consistent with the main organic matter and VOC analysis results shown. Chemical composition based on the x-ray diffraction analysis was carried out. X-ray diffraction analysis reveals the existence of chemical additive in the forms of $Ba(NO_3)_2$, $BaCO_3$, and $NaNO_3$.

• Korean Journal of Metals and Materials
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• v.47 no.5
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• pp.322-329
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• 2009

60 nm- and 20 nm-thick hydrogenated amorphous silicon (a-Si:H) layers were deposited on 200 nm $SiO_2/Si$ substrates using ICP-CVD (inductively coupled plasma chemical vapor deposition). A 10 nm-Ni layer was then deposited by e-beam evaporation. Finally, 10 nm-Ni/60 nm a-Si:H/200 nm-$SiO_2/Si$ and 10 nm-Ni/20 nm a-Si:H/200 nm-$SiO_2/Si$ structures were prepared. The samples were annealed by rapid thermal annealing for 40 seconds at $200{\sim}500^{\circ}C$ to produce $NiSi_x$. The resulting changes in sheet resistance, microstructure, phase, chemical composition and surface roughness were examined. The nickel silicide on a 60 nm a-Si:H substrate showed a low sheet resistance at T (temperatures) >$450^{\circ}C$. The nickel silicide on the 20 nm a-Si:H substrate showed a low sheet resistance at T > $300^{\circ}C$. HRXRD analysis revealed a phase transformation of the nickel silicide on a 60 nm a-Si:H substrate (${\delta}-Ni_2Si{\rightarrow}{\zeta}-Ni_2Si{\rightarrow}(NiSi+{\zeta}-Ni_2Si)$) at annealing temperatures of $300^{\circ}C{\rightarrow}400^{\circ}C{\rightarrow}500^{\circ}C$. The nickel silicide on the 20 nm a-Si:H substrate had a composition of ${\delta}-Ni_2Si$ with no secondary phases. Through FE-SEM and TEM analysis, the nickel silicide layer on the 60 nm a-Si:H substrate showed a 60 nm-thick silicide layer with a columnar shape, which contained both residual a-Si:H and $Ni_2Si$ layers, regardless of annealing temperatures. The nickel silicide on the 20 nm a-Si:H substrate had a uniform thickness of 40 nm with a columnar shape and no residual silicon. SPM analysis shows that the surface roughness was < 1.8 nm regardless of the a-Si:H-thickness. It was confirmed that the low temperature silicide process using a 20 nm a-Si:H substrate is more suitable for thin film transistor (TFT) active layer applications.

• Journal of Technologic Dentistry
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• v.29 no.1
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• pp.121-131
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• 2007

A preparation process's conditions of aqueous sol which contains anatase-type nano titania particles with photocatalyic properties was established by using Yoldas process, so called, DCS(Destabilization of Colloidal Solution) process in this study. And crystal size change and phase transformation of titania particles in aqueous titania sol depending on reaction conditions was investigated by a light scattering method and XRD analysis of frozen dried powders, respectively. This sol with photo catalytic nano titania particles was used to the following hydrophilic hybrid coating film's fabrication and its properties was evaluated. Subsequently, for coating film using the above mentioned aqueous titania sol, non-aqueous titania sol was prepared without any chemical additives and its time stability according to aging time was investigate. By using the above mentioned aqueous titania sol and non-aqueous sol, a complex oxide coating sol for metal and ceramic substrate and a organic-inorganic hybrid coating sol for polymer substrate was prepared and it's hydrophilicity depending on UV irradiation conditions was evaluated. As a conclusions, the following results were obtained. (1)Aqueous titania sol The average particle size of titania in formed aqueous titania sol was distributed between 20$\sim$90nm range depending on reaction conditions. And the crystal phase of titania powders obtained by frozen drying method was changed from amorphous state to anatase and subsequently transformed to rutile crystal phase and it is attributed to concentration gradient in aqueous sol. (2)Non-aqueous titania sol Non-aqueous titania sol was prepared using methanol as a solvent and a little distilled water for hydrolysis and nitric acid as a catalyst were used. The obtained non-aqueous titania sol was stable at room temperature for 20 days. Additionally, non-aqueous titania sol with addition of chealating reagent such as acethylaceton and ethylene glycol prolonged the stability of sol by six months. (3)Complex sol and hybrid sol with super hydrophilicity The above mentioned aqueous titania sol as a main photocataylic component and non-aqueous titania sol as a binder for coating process was used to prepare a complex sol used for metal, ceramic and wood material substrate and also to prepare the organic-inorganic hybrid sol for polymer substrate such as polycarbonate and polyethylene, in which process APMS(3-Aminopropyltrimethoxysilane), GPTS(3-Glycidoxypropyl-trimethoxysilane) as a hydrophilic silane compound and HEMA(2-Hydroxyethyl methacrylate) as a forming network in hybrid coating film were used. The hybrid coating film such as prepared through this process showed a superhydrophilicity below 1$10^{\circ}$ depending on processing conditions and a pencil's hardness over 6 H.

• Korean Journal of Optics and Photonics
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• v.16 no.2
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• pp.168-173
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• 2005

Ag-doped $TiO_2$ thin films were prepared by RF magnetron co-sputtering method, and their physical and chemical properties were examined as a function of calcination temperature. XRD results showed that the crystallite size of Ag-doped films was smaller than that of the $TiO_2$ thin films. SEM results showed that the particle size of $Ag/TiO_2$ film was smaller and more uniform than pure $TiO_2$ film. The films had high transparency in the visible range. The films calcined at $600^{\circ}C$ were the anatase phase, and the films calcined at $900^{\circ}C$ were a mixture of anatase and rutile phases. The absorption edge of films calcined at $900^{\circ}C$ was red-shifted. This is due to the augmented absorption resulting from the phase transformation from anatase to rutile phase. And the transmittance of films decreased by the light scattering and absorption in the films. Photocatalytic activity of $Ag/TiO_2$ thin films was higher than that of the pure $TiO_2$ thin films.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.24 no.2
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• pp.59-64
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• 2014

Crystallographic phases of Plasma electrolytic oxidized Al alloy, A1050, were investigated. The electrolyte of PEO was $Na_2Si_2O_3$ and KOH. Unipolar pulse, $ 2000{\mu}sec$ with $400{\mu}sec+420V$ impulse, were applied for 2 min, 5 min, 15 min, and 30 min. ${\gamma}-Alumina$, as well as ${\alpha}-alumina$, was main crystal phase. ${\gamma}-Alumina$ was appeared in the beginning, then the amount of ${\alpha}-alumina$ was increased with time, but the amount of ${\gamma}-Alumina$ remained constant without any increasing. So, it is concluded that plasma gas produce ${\gamma}-Alumina$ at the first, and then ${\gamma}-Alumina$ transform ${\alpha}-alumina$ finally. During the transformation, high temperature of micro plasma gives transformation energy.

• Korean Journal of Materials Research
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• v.20 no.9
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• pp.472-477
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• 2010

$Al_2O_3$ has received wide attention with established use as a catalyst and growing application in structural or functional ceramic materials. On the other hand, the boehmite (AlO(OH)) obtained by sol-gel process has exhibited a decrease in surface area during phase transformation due to a decline in surface active site at high temperature. In this work, $Al_2O_3$-CuO/ZnO (ACZ) and $Al_2O_3$-CuO/CeO (ACC) composite materials were synthesized with aluminum isopropoxide, copper (II) nitrate hemi (pentahydrate), and cerium (III) nitrate hexahydrate or zinc (II) nitrate hexahydrate. Moreover, the Span 80 as the template block copolymer was added to the ACZ/ACC composition to make nano size particles and to keep increasing the surface area. The ACZ/ACC synthesized powders were characterized by Thermogravimetry-Differential Thermal analysis (TG/DTA), X-ray Diffractometer (XRD), Field-Emmision Scanning Electron Microscope (FE-SEM), Bruner-Emmett-Teller (BET) surface analysis and thermal electrical conductivity (ZEM-2:M8/L). An enhancement of surface area with the addition to Span 80 surfactant was observed in the ACZ powders from 105 $m^2$/g to 142 $m^2$/g, and the ACC powders from 103 $m^2$/g to 140 $m^2$/g, respectively.

• Bulletin of the Korean Chemical Society
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• v.28 no.12
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• pp.2226-2230
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• 2007

As a cathode material of lithium rechargeable batteries, charged Li[Co0.1Ni0.15Li0.2Mn0.55]O2 electrodes, which were aged thermally at 25 oC and 90 oC respectively, were characterized by means of charge/discharger, impedance spectroscopy, and X-ray diffraction. The discharge capacity diminution of the electrodes aged at 25 oC and 90 oC for 1 week was 4% and 23%, respectively. The cell aged at 25 oC was recovered on cycling. However, the capacity loss after ageing at 90 oC was not recovered in a subsequent cycling test, which demonstrates that the reaction occurring during ageing at 90 oC is irreversible. A significant impedance increase of aged electrode at 90 oC is associated with irreversible capacity loss. The structural changes including phase transformation were not detected by XRD analysis, because it could be due to out of detection limit. After ageing, impedance was slightly decreased during subsequent cycling test. It could be explained the cyclic performance of aged sample is stable. The thermal stability was not deteriorated by ageing even at the high temperature of 90 oC.

• Journal of the Korean Ceramic Society
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• v.42 no.8 s.279
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• pp.567-574
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• 2005

Densification of SiC powder with additives of total amount of2, 4, 8 $wt\%$ Al-B-C was carried out by Spark Plasma Sintering (SPS). The unique features of the process are the possibilities of a very fast heating rate and a short holding time to obtain fully dense materials. The heating rate and applied pressure were kept at $100^{\circ}C/min$ and 40 MPa, while the sintering temperature and holding time varied from 1700 - $1800^{\circ}C$ for 10 - 40 min, respectively. The SPS-sintered specimens with different amount of Al-B-C at $1800^{\circ}C$ reached near-theoretical density. The $3C{\rightarrow}6H,\;15R{\rightarrow}4H$ phase transformation of SiC was enhanced by increasing the additive amount. The microstructure of SiC sintered up to $1750^{\circ}C$ consisted of fine equiaxed grains. In contrast, the growth of large elongated grains in small matrix grains was shown in sintered bodies at $1800^{\circ}C$, and the plate-like grains interlocking microstructure had been developed by increasing the holding time at $1800^{\circ}C$. The grain growth rate decreases with increasing amount of Al-B-C in SiC starting powder, however, the both of volume fraction and aspect ratio of large grains in sintered body increased.