• Korean Journal of Materials Research
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• v.28 no.9
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• pp.511-515
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• 2018

W-10 wt% Ti alloys that have a homogeneous microstructure are prepared by thermal decomposition of $WO_3-TiH_2$ powder mixtures and spark plasma sintering. The reduction and dehydrogenation behavior of $WO_3$ and $TiH_2$ are analyzed by temperature programmed reduction and a thermogravimetric method, respectively. The X-ray diffraction analysis of the powder mixture, heat-treated in an argon atmosphere, shows W- oxides and $TiO_2$ peaks. Conversely, the powder mixtures heated in a hydrogen atmosphere are composed of W, $WO_2$ and $TiO_2$ phases at $600^{\circ}C$ and W and W-rich ${\beta}$ phases at $800^{\circ}C$. The densified specimen by spark plasma sintering at $1500^{\circ}C$ in a vacuum using hydrogen-reduced $WO_3-TiH_2$ powder mixtures shows a Vickers hardness value of 4.6 GPa and a homogeneous microstructure with pure W, ${\beta}$ and Ti phases. The phase evolution dependent on the atmosphere and temperature is explained by the thermal decomposition and reaction behavior of $WO_3$ and $TiH_2$.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2006.04a
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• pp.19-19
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• 2006

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2005.11a
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• pp.86-86
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• 2005

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2005.04a
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• pp.30-30
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• 2005

• Journal of Powder Materials
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• v.10 no.6
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• pp.422-429
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• 2003

The reduction mechanism of the composite powders mixed with $WO_3$ and CuO has been studied by using thermogravimetry (TG), X-ray diffraction, and microstructure analyses. The composite powders were made by simple Turbula mixing, spray drying, and ball-milling in a stainless steel jar with the ball to powder ratio of 32 to 1 at 80 rpm for 1 h without process controlling agents. It is observed that all the oxide composite powders are converted to W-coated Cu composite powder after reducing treatment under hydrogen atmosphere. For the formation mechanism of W-coated Cu composite powder, the sequential reduction steps are proposed as follows: CuO contained in the ball-milled composite powder is initially reduced to Cu at the temperature range from 20$0^{\circ}C$ to 30$0^{\circ}C$. Then, $WO_3$ powder is reduced to W $O_2$ via W $O_{2.9}$ and W $O_{2.72}$ at higher temperature region. Finally, the gaseous phase of $WO_3(OH)_2$ formed by reaction of $WO_2$ with water vapour migrates to previously reduced Cu and deposits on it as W reduced by hydrogen. The proposed mechanism has been proved through the model experiment which was performed by using Cu plate and $WO_3$ powder.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2003.04a
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• pp.24-24
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• 2003

• Journal of Powder Materials
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• v.19 no.4
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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.

• Journal of Powder Materials
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• v.24 no.1
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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.

• Journal of Powder Materials
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• v.25 no.3
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• pp.240-245
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• 2018

This study focuses on the fabrication of a WC/Co composite powder from the oxide of WC/Co hardmetal scrap using solid carbon in a hydrogen gas atmosphere for the recycling of WC/Co hardmetal. Mixed powders are manufactured by mechanically milling the oxide powder of WC-13 wt% Co hardmetal scrap and carbon black with varying powder/ball weight ratios. The oxide powder of WC-13 wt% Co hardmetal scrap consists of $WO_3$ and $CoWO_4$. The mixed powder mechanically milled at a lower powder/ball weight ratio (high mechanical milling energy) has a more rapid carbothermal reduction reaction in the formation of WC and Co phases compared with that mechanically milled at a higher powder/ball weight ratio (lower mechanical milling energy). The WC/Co composite powder is fabricated at $900^{\circ}C$ for 6 h from the oxide of WC/Co hardmetal scrap using solid carbon in a hydrogen gas atmosphere. The fabricated WC/Co composite powder has a particle size of approximately $0.25-0.5{\mu}m$.

• Korean Journal of Materials Research
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• v.25 no.11
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• pp.602-606
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• 2015

Porous W with spherical and directionally aligned pores was fabricated by the combination of sacrificial fugitives and a freeze-drying process. Camphene slurries with powder mixtures of $WO_3$ and spherical PMMA of 20 vol% were frozen at $-25^{\circ}C$ and dried for the sublimation of the camphene. The green bodies were heat-treated at $400^{\circ}C$ for 2 h to decompose the PMMA; then, sintering was carried out at $1200^{\circ}C$ in a hydrogen atmosphere for 2 h. TGA and XRD analysis showed that the PMMA decomposed at about $400^{\circ}C$, and $WO_3$ was reduced to metallic W at $800^{\circ}C$ without any reaction phases. The sintered bodies with $WO_3$-PMMA contents of 15 and 20 vol% showed large pores with aligned direction and small pores in the internal walls of the large pores. The pore formation was discussed in terms of the solidication behavior of liquid camphene with solid particles. Spherical pores, formed by decomposition of PMMA, were observed in the sintered specimens. Also, microstructural observation revealed that struts between the small pores consisted of very fine particles with size of about 300 nm.