• Journal of Powder Materials
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• v.13 no.3 s.56
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• pp.205-210
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• 2006

The effect of Cu content on hydrogen reduction behavior of ball-milled $WO_3$-CuO nanocomposite powders was investigated. Hydrogen reduction behavior and reduction percent(${\alpha}$) of nanopowders were characterized by thermogravimetry (TG) and hygrometry measurements. Activation energy for hydrogen reduction of $WO_3$ nanopowders with different Cu content was calculated at each heating rate and reduction percent(${\alpha}$). The activation energy for reduction of $WO_3$ obtained in this study existed in the ranging from 129 to 139 kJ/mol, which was in accordance with the activation energy for $WO_3$ powder reduction of conventional micron-sized.

• Korean Journal of Metals and Materials
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• v.47 no.9
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• pp.597-603
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• 2009

The hydrogen reduction behavior of ultrasonic ball-milled $WO_3-CuO$ nanopowder, which is highly related with micro-pore structure, was investigated by thermogravimetry(TG) and hygrometry system. EDS and TEM results represented that the ultrasonic ball-milled $WO_3-CuO$ nanopowder consisted of the agglomerates which was confirmed as a homogeneous mixture of $WO_3$ and CuO particles. It was found that the reduction reaction of CuO was retarded by initial micro-pores which are smaller than 40 nm in the ultrasonic ball-milled $WO_3-CuO$ nanopowder. The earlier agglomeration of Cu particles at comparably low temperature decreased the volume of micro-pores in the $WO_3-CuO$ nanopowder which caused the retardation of $WO_3$ reduction reaction. These results clearly explain that the micro-pore structure significantly affected the reduction reaction of $WO_3$ and CuO in the $WO_3-CuO$ nanopowder.

• Korean Journal of Materials Research
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• v.13 no.9
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• pp.631-634
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• 2003

To fabricate W-Cu nanocomposite powder, $WO_3$-CuO powder mixture was high-energetically ball-milled and subsequently hydrogen-reduced. The effect of ball-milling on the hydrogen-reduction behavior of$ WO_3$-CuO was investigated with non-isothermal hygrometric analysis during hydrogen-reduction. Increasing the ball-milling time, the reduction peak temperatures of humidity curves were shifted to low temperature. It was considered that the reduction temperature should be decreased because the specific surface area of each oxide considerably increased with increasing the ball-milling time. In case of ball-milling for 0 h, $WO_3$and CuO were independently hydrogen-reduced and W particles were nucleated on the surface of Cu adjacent to W by CVT. However, in case of ball-milling for 50 h, the aggregates of about 200-300 nm were observed. W particles of size below 30-50 nm were homogeneously distributed with Cu in the aggregates.

• Korean Journal of Materials Research
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• v.27 no.10
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• pp.513-517
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• 2017

An optimum route to fabricate a hybrid-structured W powder composed of nano and micro size powders was investigated. The mixture of nano and micro W powders was prepared by a ball milling and hydrogen reduction process for $WO_3$ and W powders. Microstructural observation for the ball-milled powder mixtures revealed that the nano-sized $WO_3$ particles were homogeneously distributed on the surface of large W powders. The reduction behavior of $WO_3$ powder was analyzed by a temperature programmed reduction method with different heating rates in Ar-10% $H_2$ atmosphere. The activation energies for the reduction of $WO_3$, estimated by the slope of the Kissinger plot from the amount of reaction peak shift with heating rates, were measured as 117.4 kJ/mol and 94.6 kJ/mol depending on reduction steps from $WO_3$ to $WO_2$ and from $WO_2$ to W, respectively. SEM and XRD analysis for the hydrogen-reduced powder mixture showed that the nano-sized W particles were well distributed on the surface of the micro-sized W powders.

• Transactions of the Korean hydrogen and new energy society
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• v.22 no.4
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• pp.443-450
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• 2011

The three-reactor chemical-looping process (TRCL) for the production of hydrogen from natural gas is attractive for both $CO_2$ capture and hydrogen production. In this study, redox property of $Fe_2O_3$ and $WO_3$ supported with $ZrO_2$ and $MgAl_2O_4$ were studied with temperature programmed oxidation/reduction (TPO/R) experiment. All metal oxides were prepared by ball mill method. Metal oxides supported with $ZrO_2$ showed the good redox property in TPO and TPR tests. Reduction behavior was matched well the theoretical reduction mechanism. Metal oxides supported with $MgAl_2O_4$ formed a solid solution ($MgFe_{0.6}Al_{1.4}O_4$, $MgWO_4$). $Fe_2O_3$ showed more narrow reaction range and lower reaction temperature than $WO_3$.

• Journal of Powder Materials
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• v.24 no.6
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• pp.472-476
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• 2017

Porous W-10 wt% Ti alloys are prepared by freeze-drying a $WO_3-TiH_2$/camphene slurry, using a sintering process. X-ray diffraction analysis of the heat-treated powder in an argon atmosphere shows the $WO_3$ peak of the starting powder and reaction-phase peaks such as $WO_{2.9}$, $WO_2$, and $TiO_2$ peaks. In contrast, a powder mixture heated in a hydrogen atmosphere is composed of the W and TiW phases. The formation of reaction phases that are dependent on the atmosphere is explained by a thermodynamic consideration of the reduction behavior of $WO_3$ and the dehydrogenation reaction of $TiH_2$. To fabricate a porous W-Ti alloy, the camphene slurry is frozen at $-30^{\circ}C$, and pores are generated in the frozen specimens by the sublimation of camphene while drying in air. The green body is hydrogen-reduced and sintered at $1000^{\circ}C$ for 1 h. The sintered sample prepared by freeze-drying the camphene slurry shows large and aligned parallel pores in the camphene growth direction, and small pores in the internal walls of the large pores. The strut between large pores consists of very fine particles with partial necking between them.

• Journal of Powder Materials
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• v.24 no.5
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• pp.384-388
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• 2017

The effect of the mixing method on the characteristics of hybrid-structure W powder with nano and micro sizes is investigated. Fine $WO_3$ powders with sizes of ${\sim}0.6{\mu}m$, prepared by ball milling for 10 h, are mixed with pure W powder with sizes of $12{\mu}m$ by various mixing process. In the case of simple mixing with ball-milled $WO_3$ and micro sized W powders, $WO_3$ particles are locally present in the form of agglomerates in the surface of large W powders, but in the case of ball milling, a relatively uniform distribution of $WO_3$ particles is exhibited. The microstructural observation reveals that the ball milled $WO_3$ powder, heat-treated at $750^{\circ}C$ for 1 h in a hydrogen atmosphere, is fine W particles of ~200 nm or less. The powder mixture prepared by simple mixing and hydrogen reduction exhibits the formation of coarse W particles with agglomeration of the micro sized W powder on the surface. Conversely, in the powder mixture fabricated by ball milling and hydrogen reduction, a uniform distribution of fine W particles forming nano-micro sized hybrid structure is observed.

• Korean Journal of Materials Research
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• v.28 no.2
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• pp.108-112
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• 2018

The present study demonstrates the effect of raw powder on the pore structure of porous W-Ni prepared by freeze drying of camphene-based slurries and sintering process. The reduction behavior of $WO_3$ and $WO_3-NiO$ powders is analyzed by a temperature programmed reduction method in Ar-10% H2 atmosphere. After heat treatment in hydrogen atmosphere, $WO_3-NiO$ powder mixture is completely converted to metallic W without any reaction phases. Camphene slurries with oxide powders are frozen at $-30^{\circ}C$, and pores in the frozen specimens are generated by sublimation of the camphene during drying in air. The green bodies are hydrogen-reduced at $800^{\circ}C$ and sintered at $1000^{\circ}C$ for 1 h. The sintered samples show large and aligned parallel pores to the camphene growth direction, and small pores in the internal wall of large pores. The strut between large pores, prepared from pure $WO_3$ powder, consists of very fine particles with partially necking between the particles. In contrast, the strut densification is clearly observed in the Ni-added W sample due to the enhanced mass transport in activation sintering.

• Journal of Powder Materials
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• v.24 no.1
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• pp.41-45
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• 2017

The effects of the heat treatment temperature and of the atmosphere on the dehydrogenation and hydrogen reduction of ball-milled $TiH_2-WO_3$ powder mixtures are investigated for the synthesis of Ti-W powders with controlled microstructure. Homogeneously mixed powders with refined $TiH_2$ particles are successfully prepared by ball milling for 24h. X-ray diffraction (XRD) analyses show that the powder mixture heat-treated in Ar atmosphere is composed of Ti, $Ti_2O$, and W phases, regardless of the heat treatment temperature. However, XRD results for the powder mixture, heat-treated at $600^{\circ}C$ in a hydrogen atmosphere, show $TiH_2$ and TiH peaks as well as reaction phase peaks of Ti oxides and W, while the powder mixture heat-treated at $900^{\circ}C$ exhibits only XRD peaks attributed to Ti oxides and W. The formation behavior of the reaction phases that are dependent on the heat treatment temperature and on the atmosphere is explained by thermodynamic considerations for the dehydrogenation reaction of $TiH_2$, the hydrogen reduction of $WO_3$ and the partial oxidation of dehydrogenated Ti.

• Journal of Powder Materials
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• v.22 no.2
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• pp.129-133
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• 2015

Porous W with controlled pore structure was fabricated by thermal decomposition and hydrogen reduction process of PMMA beads and $WO_3$ powder compacts. The PMMA sizes of 8 and $50{\mu}m$ were used as pore forming agent for fabricating the porous W. The $WO_3$ powder compacts with 20 and 70 vol% PMMA were prepared by uniaxial pressing and sintered for 2 h at $1200^{\circ}C$ in hydrogen atmosphere. TGA analysis revealed that the PMMA was decomposed at about $400^{\circ}C$ and $WO_3$ was reduced to metallic W at $800^{\circ}C$. Large pores in the sintered specimens were formed by thermal decomposition of spherical PMMA, and their size was increased with increase in PMMA size and the amount of PMMA addition. Also the pore shape was changed from spherical to irregular form with increasing PMMA contents due to the agglomeration of PMMA in the powder mixing process.