• Journal of Powder Materials
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• 제21권1호
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• pp.34-38
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• 2014

Cu-Ni alloys with unidirectionally aligned pores were prepared by freeze-drying process of CuO-NiO/camphene slurry. Camphene slurries with dispersion stability by the addition of oligomeric polyester were frozen at $-25^{\circ}C$, and pores in the frozen specimens were generated by sublimation of the camphene during drying in air. The green bodies were hydrogen-reduced at $300^{\circ}C$ and sintered at $850^{\circ}C$ for 1 h. X-ray diffraction analysis revealed that CuO-NiO composite powders were completely converted to Cu-Ni alloy without any reaction phases by hydrogen reduction. The sintered samples showed large and aligned parallel pores to the camphene growth direction, and small pores in the internal wall of large pores. The pore size and porosity decreased with increase in CuO-NiO content from 5 to 10 vol%. The change of pore characteristics was explained by the degree of powder rearrangement in slurry and the accumulation behavior of powders in the interdendritic spaces of solidified camphene.

• Korean Journal of Materials Research
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• 제23권12호
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• pp.722-726
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• 2013

Freeze drying of a porous Cu-Sn alloy with unidirectionally aligned pore channels was accomplished by using a composite powder of CuO-$SnO_2$ and camphene. Camphene slurries with CuO-$SnO_2$ content of 3, 5 and 10 vol% were prepared by mixing with a small amount of dispersant at $50^{\circ}C$. Freezing of a slurry was done 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 bodies were hydrogen-reduced at $650^{\circ}C$ and then were sintered at $650^{\circ}C$ and $750^{\circ}C$ for 1 h. XRD analysis revealed that the CuO-$SnO_2$ powder was completely converted to Cu-Sn alloy without any reaction phases. The sintered samples showed large pores with an average size of above $100{\mu}m$ which were aligned parallel to the camphene growth direction. Also, the internal walls of the large pores had relatively small pores. The size of the large pores decreased with increasing CuO-$SnO_2$ content due to the change of the degree of powder rearrangement in the slurry. The size of the small pores decreased with increase of the sintering temperature from $650^{\circ}C$ to $750^{\circ}C$, while that of the large pores was unchanged. These results suggest that a porous alloy body with aligned large pores can be fabricated by a freeze-drying and hydrogen reduction process using oxide powders.

• Korean Journal of Materials Research
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• 제19권5호
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• pp.270-275
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• 2009

Lotus-type porous nickel with cylindrical pores was fabricated by unidirectional solidification under an Ar gas atmosphere using the thermal decomposition method of the compounds such as sodium hydroxide, calcium hydroxide, calcium carbonate, and titanium hydride. The decomposed gas does form the pores in liquid nickel, and then, the pores become the cylindrical pores during unidirectional solidification. The decomposed particles from the compounds do play a rule on nucleation sites of the pores. The behavior of pore growth was controlled by atmosphere pressure, which can be explained by Boyle's law. The porosity and pore size decreased with increasing Ar gas pressure when the pores contain hydrogen gas decomposed from calcium and sodium hydroxide and titanium hydride, ; however it they did not change when the pores contain containing carbon dioxide decomposed from calcium carbonate. These results indicate that nickel does not have the solubility of carbon dioxide. Lotus-type porous metals can be easily fabricated by the thermal decomposition method, which is superior to the conventional fabrication method used to pressurized gas atmospheres.

• Journal of Powder Materials
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• 제19권6호
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• pp.446-450
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• 2012

In order to fabricate the porous Mo with controlled pore characteristics, unique processing by using $MoO_3$ powder as the source and camphene as the sublimable material is introduced. Camphene-based 15 vol% $MoO_3$ slurries, prepared by milling at $50^{\circ}C$ with a small amount of dispersant, were frozen 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 $750^{\circ}C$, and sintered at $1000-1100^{\circ}C$ for 1 h. After heat treatment in hydrogen atmosphere, $MoO_3$ powders were completely converted to metallic W without any reaction phases. The sintered samples showed large pores with the size of about $150{\mu}m$ 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 due to the difference in the camphene growth rate during freezing process. The size of small pores was decreased with increase in sintering temperature, while that of large pores was unchanged. The results are strongly suggested that the porous metal with required pore characteristics can be successfully fabricated by freeze-drying process using metal oxide powders.

• Journal of Powder Materials
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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.

• Korean Journal of Materials Research
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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.

• Journal of Powder Materials
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• 제26권1호
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• pp.1-5
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• 2019

In this study, porous Mo-5 wt% Cu with unidirectionally aligned pores is prepared by freeze drying of camphene slurry with $MoO_3-CuO$ powders. Unidirectional freezing of camphene slurry with dispersion stability is conducted at $-25^{\circ}C$, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The green bodies are hydrogen-reduced at $750^{\circ}C$ and sintered at $1000^{\circ}C$ for 1 h. X-ray diffraction analysis reveals that $MoO_3-CuO$ composite powders are completely converted to a Mo-and-Cu phase without any reaction phases by hydrogen reduction. The sintered bodies with the Mo-Cu phase show large and aligned parallel pores to the camphene growth direction as well as small pores in the internal walls of large pores. The pore size and porosity decrease with increasing composite powder content from 5 to 10 vol%. The change of pore characteristics is explained by the degree of powder rearrangement in slurry and the accumulation behavior of powders in the interdendritic spaces of solidified camphene.

• Journal of Powder Materials
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• 제27권3호
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• pp.193-197
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• 2020

Porous Cu-14 wt% Co with aligned pores is produced by a freeze drying and sintering process. Unidirectional freezing of camphene slurry with CuO-Co₃O₄ powders is conducted, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The dried bodies are hydrogen-reduced at 500℃ and sintered at 800℃ for 1 h. The reduction behavior of the CuO-Co₃O₄ powder mixture is analyzed using a temperature-programmed reduction method in an Ar-10% H₂ atmosphere. The sintered bodies show large and aligned parallel pores in the camphene growth direction. In addition, small pores are distributed around the internal walls of the large pores. The size and fraction of the pores decrease as the amount of solid powder added to the slurry increases. The change in pore characteristics according to the amount of the mixed powder is interpreted to be due to the rearrangement and accumulation behavior of the solid particles in the freezing process of the slurry.

• Journal of Powder Materials
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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.

• Journal of Powder Materials
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• 제26권1호
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• pp.6-10
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• 2019

In this study, freeze drying of a porous Ni with unidirectionally aligned pore channels is accomplished by using a NiO powder and camphene. Camphene slurries with NiO content of 5 and 10 vol% are prepared by mixing them with a small amount of dispersant at $50^{\circ}C$. Freezing of a slurry is performed at $-25^{\circ}C$ while the growth direction of the camphene is unidirectionally controlled. Pores are generated subsequently by sublimation of the camphene during drying in air for 48 h. The green bodies are hydrogen-reduced at $400^{\circ}C$ and then sintered at $800^{\circ}C$ and $900^{\circ}C$ for 1 h. X-ray diffraction analysis reveals that the NiO powder is completely converted to the Ni phase without any reaction phases. The sintered samples show large pores that align parallel pores in the camphene growth direction as well as small pores in the internal walls of large pores. The size of large and small pores decreases with increasing powder content from 5 to 10 vol%. The influence of powder content on the pore structure is explained by the degree of powder rearrangement in slurry and the accumulation behavior of powders in the interdendritic spaces of solidified camphene.