• 대한화학회지
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• 제67권1호
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• pp.33-41
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• 2023

Nanocrystallne WO₃ and MoO₃ with several different sizes and crystal structures were prepared by simple acid precipitation and subsequent heat treatment. The photochromic (PC) properties of these samples were comparatively investigated in powder state by monitoring diffuse reflectance spectral changes after bandgap irradiation. The PC effect of hexagonal WO₃ and monoclinic WO₃ strongly depended upon crystallite size rather than crystal structure. The smaller the crystallite size, the better the PC effect. However, orthorhombic WO·H₂O and MoO₃ having hexagonal and orthorhombic structures did not follow this trend. One consistent result for all WO₃ and MoO₃ samples is that the heat treatment in air, which changes crystallinity, whether it changes the crystal structure or only the crystallite size, reduces the PC effect. Since the thermal treatment reduces the surface oxygen defect sites, we believe that the PC effect of WO₃ and MoO₃ depends critically on the surface oxygen defect sites that serve as deep trap sites for photogenerated electrons and oxygen radical holes. We also found that the proton insertion claimed by double charge injection model is not critical for the PC effect.

• 한국분말재료학회지
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• 제19권4호
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• pp.259-263
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• 2012

Dependence of the freeze-drying process condition on microstructure of porous W and pore formation mechanism were studied. Camphene slurries with $WO_3$ contents of 10 vol% were prepared by milling at $50^{\circ}C$ with a small amount of dispersant. Freezing of a slurry was done in Teflon cylinder attached to a copper bottom plate cooled at $-25^{\circ}C$. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green body was hydrogen-reduced at $800^{\circ}C$ for 30 min, and sintered in the furnace at $900^{\circ}C$ for 1 h. After heat treatment in hydrogen atmosphere, $WO_3$ powders were completely converted to metallic W without any reaction phases. The sintered samples showed large pores with the size of about $70{\mu}m$ which were aligned parallel to the camphene growth direction. Also, the internal wall of large pores and near bottom part of specimen had relatively small pores with dendritic structure due to the growth of camphene dendrite depending on the degree of nucleation and powder rearrangement in the slurry.

• 한국재료학회지
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• 제21권6호
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• pp.299-302
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• 2011

[ $WO_3$ ]powders were ball-milled with an alumina ball for 0-72 hours. $In_2O_3$ doped $WO_3$ was prepared by soaking ball-milled $WO_3$ in an $InCl_3$ solution. The mixed powder was annealed at $700^{\circ}C$ for 30 min in an air atmosphere. A paste for screen-printing the thick film was prepared by mixing the $WO_3$:In2O3 powders with ${\alpha}$-terpinol and glycerol. $In_2O_3$ doped $WO_3$ thick films were fabricated into a gas sensor by a screen-printing method on alumina substrates. The structural properties of the $WO_3$:$InO_3$ thick films were a monoclinic phase with a (002) dominant orientation. The particle size of the $WO_3$:$InO_3$ decreased with the ball-milling time. The sensing characteristics of the $In_2O_3$ doped $WO_3$ were investigated by measuring the electrical resistance of each sensor in the test-box. The highest sensitivity to 5 ppm $CH_4$ gas and 5 ppm $CH_3CH_2CH_3$ gas was observed in the ball-milled $WO_3$:$InO_3$ gas sensors at 48 hours. The response time of $WO_3$:$In_2O_3$ gas sensors was 7 seconds and recovery time was 9 seconds for the methane gas.

• 대한전기학회:학술대회논문집
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• 대한전기학회 1998년도 하계학술대회 논문집 D
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• pp.1346-1348
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• 1998

Tungsten oxide($WO_3$) thin films were prepared by reactive magnetron sputtering in an $Ar/O_2$ atmosphere from a compressed powder $WO_3$ target and their electrochromic(EC) phenomena were investigated. PEO-$LiClO_4$-PC polymer electrolyte can easely be formed into thin films and showed high transmittance. Such electrolyte have electrochromic properties suitable for large-scale electrochromic devices. For the devices using $WO_3$ thin films of 1500, 2500, $4000{\AA}$ thickness with glass/ITO/$WO_3$/PEO-$LiClO_4$-PC/ITO/glass structure, an optical modulation of $50{\sim}60%$ were obtained at a potential range of $1{\sim}2V$. It has shown that transmittance and reflectance of light could be electrically controlled by low applied voltage.

• 한국분말재료학회지
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• 제29권2호
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• pp.118-122
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• 2022

The synthesis of porous W by freeze-casting and vacuum drying is investigated. Ball-milled WO₃ powders and tert-butyl alcohol were used as the starting materials. The tert-butyl alcohol slurry is frozen at -25℃ and dried under vacuum at -25 and -10℃. The dried bodies are hydrogen-reduced at 800℃ and sintered at 1000℃. The XRD analysis shows that WO₃ is completely reduced to W without any reaction phases. SEM observations reveal that the struts and pores aligned in the tert-butyl alcohol growth direction, and the change in the powder content and drying temperature affects the pore structure. Furthermore, the struts of the porous body fabricated under vacuum are thinner than those fabricated under atmospheric pressure. This behavior is explained by the growth mechanism of tert-butyl alcohol and rearrangement of the powders during solidification. These results suggest that the pore structure of a porous body can be controlled by the powder content, drying temperature, and pressure.

• 한국분말재료학회지
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• 제12권2호
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• pp.112-116
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• 2005

In the present study, the focus is on the analysis of carbothermal reduction of oxide powder prepared from waste WC/Co hardmetal by solid carbon under a stream of argon for the recycling of the WC/Co hard-metal. The oxide powder was prepared by the combination of the oxidation and crushing processes using the waste $WC-8 wt.\%Co$ hardmetal as the raw material. This oxide powder was mixed with carbon black, and then this mixture was carbothermally reduced under a flowing argon atmosphere. The changes in the phase structure and gases discharge of the mixture during carbothermal reduction was analysed using XRD and gas analyzer. The oxide powder prepared from waste $WC-8wt.\%Co$ hardmetal has a mixture of $WO_{3} and CoWO_{4}$. This oxide powder reduced at about $850^{\circ}C$, formed tungsten carbides at about $950^{\circ}C$, and then fully transformed to a mixed state of tungsten carbide (WC) and cobalt at about $1100^{\circ}C$ by solid carbon under a stream of argon. The WC/Co composite powder synthesized at $1000^{\circ}C$ for 6 hours from oxide powder of waste $WC-8wt.\%Co$ hardmetal has an average particle size of $0.3 {\mu}m$.

• 한국분말재료학회지
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• 제24권1호
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• pp.34-40
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• 2017

This study is carried out to obtain basic data regarding oxidation and reduction reactions, originated on the recycling of waste tungsten hard scraps by oxidation and reduction processes. First, it is estimated that the theoretical Gibbs free energy for the formation reaction of $WO_2$ and $WO_3$ are calculated as ${\Delta}G_{1,000K}=-407.335kJ/mol$ and ${\Delta}G_{1,000K}=-585.679kJ/mol$, from the thermodynamics data reported by Ihsan Barin. In the experiments, the oxidation of pure tungsten rod by oxygen is carried out over a temperature range of $700-1,000^{\circ}C$ for 1 h, and it is possible to conclude that the oxidation reaction can be represented by a relatively linear relationship. Second, the reduction of $WO_2$ and $WO_3$ powder by hydrogen is also calculated from the same thermodynamics data, and it can be found that it was difficult for the reduction reaction to occur at $1,027^{\circ}C$, in the case of $WO_2$, but it can happen for temperatures higher than $1127^{\circ}C$. On the other hand, $WO_3$ reduction reaction occurs at the relatively low temperature of $827^{\circ}C$. Based on these results, the reduction experiments are carried out at a temperature range of $500-1,000^{\circ}C$ for 15 min to 4 h, in the case of $WO_3$ powder, and it is possible to conclude that the reduction at $900^{\circ}C$ for 2h is needed for a perfect reduction reaction.

• 한국세라믹학회지
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• 제44권3호
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• pp.152-156
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• 2007

Tungsten carbide powder was synthesized by SHS (self-propagating high-temperature synthesis). Except $WO_{3}$, each concentration of raw material ($WO_{3},\;Mg,\;NaCl,\;Na_{2}CO_{3},\;C$) was investigated. Final product was characterized by XRD and SEM. X-ray data demonstrated that the $NaCl+Na_{2}CO_{3}$ combined mixture has superiority in the WC formation process. Single phase and submicrometer WC powder was synthesized at the temperature below $1600^{\circ}C$. The role of sodium salts in combustion process was discussed, and chemical mechanism of WC formation was proposed. WC powder prepared by salt-assisted combustion synthesis has a size $0.2{\sim}3\;{\mu}m$ and low agglomeration degree.

• 한국전기전자재료학회논문지
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• 제27권8호
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• pp.510-515
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• 2014

Thin films of cubic $Na_{0.6}WO_3$, which is one of the sodium tungsten bronze, were fabricated by rf sputtering for the electrode applications in integrated sensors and actuators. A single-phase cubic $Na_{0.6}WO_3$ sputtering target of power type was prepared by conventional solid-state reaction. Thin films were deposited from the powder target, and the as-deposited films were amorphous, thus they annealed by tube furnace or RTP for crystallization. Thin films having cubic phase $Na_xWO_3$ were fabricated by the optimization of sputtering and post-annealing conditions, but single-phase cubic $Na_{0.6}WO_3$ thin films were not obtained. Although the films were not in single phase, they had good electrical conduction properties showing electrical resistivities of $10-4{\Omega}{\cdot}cm$ order.

• 한국전기전자재료학회논문지
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• 제25권8호
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• pp.602-610
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• 2012

The powders for the $Na_xWO_3$ (x= 1 and 0.75) sputtering targets were synthesized by the calcination in reductive atmosphere. Near single-phase $NaWO_3$ and single-phase $Na_{0.75}WO_3$ powder targets were prepared. By using the targets, thin films of each composition were deposited by rf magnetron sputtering on the $SiO_2$ (100 nm)/Si substrates and annealed by RTP (rapid thermal processing) for crystallization. In the case of the $NaWO_3$ composition, single-phase $Na_xWO_3$ thin films, where x was believed to be slightly less than 1, were fabricated accompanying the Na-diffusion into the substrates during RTP. However, in the case of the $Na_{0.75}WO_3$ thin film preparation, it was unable to make single-phase thin films. From the phase formation behaviors of both powders and thin films, it was revealed that $Na_xWO_3$ with nonstoichiometric composition of x, which was slightly less than 1, was favorable. The good electrical conduction properties were obtained from the single-phase $Na_xWO_3$ thin films. Their electrical resistivities were as low as $7.5{\times}10^{-4}{\Omega}{\cdot}cm$.