• 한국분말재료학회지
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• 제24권6호
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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.

• 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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• 제21권9호
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• pp.520-524
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• 2011

Porous W with controlled pore characteristics was fabricated by a freeze-drying process. $WO_3$ powder and camphene were used as the source materials of W and sublimable vehicles, respectively. Camphene slurries with $WO_3$ contents of 10 and 15 vol% were prepared by milling at $50^{\circ}C$ with a small amount of oligomeric polyester dispersant. Freezing of a slurry was done in a Teflon cylinder attached to a copper bottom plate cooled at $-25^{\circ}C$ while the growth direction of the camphene was unidirectionally controlled. 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 a furnace at $900^{\circ}C$ for 1 h under a hydrogen atmosphere. Microstructural observation revealed that all of the sintered samples were composed of only W phase and showed large pores which were aligned parallel to the camphene growth direction. The porosity and pore size increased with increasing camphene content. The difference in the pore characteristics depending on the slurry concentration may be explained by the degree of powder rearrangement in the slurry. The results strongly suggest that a porous metal with the required pore characteristics can be successfully fabricated by a freeze-drying process using metal oxide powders.

• 한국재료학회지
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• 제28권2호
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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.