• Korean Journal of Materials Research
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• v.23 no.6
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• pp.339-343
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• 2013

Porous Ti-systems with unidirectionally aligned channels were synthesized by freeze-drying and a heat treatment process. $TiH_2$ powder and camphene were used as the source materials of Ti and sublimable vehicles, respectively. Camphene slurries with $TiH_2$ content of 10 and 15 vol% were prepared by milling at $50^{\circ}C$ with a small amount of oligomeric polyester dispersant. Freezing of the slurry was done in a Teflon cylinder attached to a copper bottom plate cooled at $-25^{\circ}C$ while unidirectionally controlling the growth direction of the camphene. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green body was heat-treated at $1100^{\circ}C$ for 1 h in a nitrogen and air atmosphere. XRD analysis revealed that the samples composed of TiN and $TiO_2$ phase were dependent on the heat-treatment atmosphere. The sintered samples showed large pores of about 120 mm which were aligned parallel to the camphene growth direction. The internal wall of the large pores had relatively small pores with a dendritic structure due to the growth of camphene dendrite depending on the degree of nucleation and powder rearrangement in the slurry. These results suggest that a porous body with an appropriate microstructure can be successfully fabricated by freeze-drying and a controlled sintering process of a camphene/$TiH_2$ slurry.

• Journal of Powder Materials
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• v.26 no.1
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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.

• Journal of Powder Materials
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• v.19 no.6
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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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• v.21 no.1
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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.

• Journal of Powder Materials
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• v.18 no.4
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• pp.327-331
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• 2011

In order to fabricate the porous metal with controlled pore characteristics, unique processing by using metal oxide powder as the source and camphene as the sublimable material is introduced. CuO powder was selected as the source for the formation of Cu metal via hydrogen reduction. Camphene-based CuO slurry, prepared by milling at $47^{\circ}C$ with a small amount of dispersant, was frozen at $-25^{\circ}C$. Pores were generated subsequently by sublimation of the camphene. The green body was hydrogen-reduced at $200^{\circ}C$ for 30 min, and sintered at $500-700^{\circ}C$ for 1 h. Microstructural analysis revealed that the sintered Cu showed aligned large pore channels parallel to the camphene growth direction, and fine pores are formed around the large pore. Also, it showed that the pore size was controllable by the slurry concentration.

• Journal of Powder Materials
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• v.22 no.6
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• pp.438-442
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• 2015

Porous thick film of alumina which is fabricated by freeze tape casting using a camphene-camphor-acrylate vehicle. Alumina slurry is mixed above the melting point of the camphene-camphor solvent. Upon cooling, the camphene-camphor crystallizes from the solution as particle-free dendrites, with the $Al_2O_3$ powder and acrylate liquid in the interdendritic spaces. Subsequently, the acrylate liquid is solidified by photopolymerization to offer mechanical properties for handling. The microstructure of the porous alumina film is characterized for systems with different cooling rate around the melting temperature of camphor-camphene. The structure of the dendritic porosity is compared as a function of ratio of camphene-camphor solvent and acrylate content, and $Al_2O_3$ powder volume fraction in acrylate in terms of the dendrite arm width.

• Journal of Powder Materials
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• v.21 no.3
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• pp.191-195
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• 2014

This study reports a simple way of fabricating the porous Cu with unidirectional pore channels by freeze drying camphene slurry with Cu oxide coated Cu powders. The coated powders were prepared by calcination of ball-milled powder mixture of Cu and Cu-nitrate. Improved dispersion stability of camphene slurry could be achieved using the Cu oxide coated Cu powders instead of pure Cu powders. Pores in the frozen specimen at $-25^{\circ}C$ were generated by sublimation of the camphene during drying in air, and the green bodies were sintered at $750^{\circ}C$ for 1 h in $H_2$ atmosphere. XRD analysis revealed that the coated layer of Cu oxide was completely converted to Cu phase without any reaction phases by hydrogen heat treatment. The porous Cu specimen prepared from pure Cu powders showed partly large pores with unidirectional pore channels, but most of pores were randomly distributed. In contrast, large and aligned parallel pores to the camphene growth direction were clearly observed in the sample using Cu oxide coated Cu powders. Pore formation behavior depending on the initial powders was discussed based on the degree of powder rearrangement and dispersion stability in slurry.

• Journal of Powder Materials
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• v.23 no.1
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• pp.49-53
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• 2016

The present study demonstrates the effect of freezing conditions on the pore structure of porous Cu-10 wt.% Sn prepared by freeze drying of $CuO-SnO_2$/camphene slurry. Mixtures of CuO and $SnO_2$ powders are prepared by ball milling for 10 h. Camphene slurries with 10 vol.% of $CuO-SnO_2$ are unidirectionally frozen in a mold maintained at a temperature of $-30^{\circ}C$ for 1 and 24 h, respectively. Pores are generated by the sublimation of camphene at room temperature. After hydrogen reduction and sintering at $650^{\circ}C$ for 2 h, the green body of the $CuO-SnO_2$ is completely converted into porous Cu-Sn alloy. Microstructural observation reveals that the sintered samples have large pores which are aligned parallel to the camphene growth direction. The size of the large pores increases from 150 to $300{\mu}m$ with an increase in the holding time. Also, the internal walls of the large pores contain relatively small pores whose size increases with the holding time. The change in pore structure is explained by the growth behavior of the camphene crystals and rearrangement of the solid particles during the freezing process.

• Korean Journal of Materials Research
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• v.21 no.9
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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.

• Korean Journal of Materials Research
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• v.25 no.1
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• pp.27-31
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• 2015

This paper proposes a novel way of fabricating aligned porous Sn by freeze-drying of camphene slurry with stannic oxide ($SnO_2$) coated Sn powders. The $SnO_2$ coated Sn powders were prepared by surface oxidation of the initial and ball-milled Sn powders, as well as heat treatment of tin chloride coated Cu powders. Camphene slurries with 10 vol% solid powders were prepared by mixing at $50^{\circ}C$ with a small amount of oligomeric polyester dispersant. Freezing the slurry was done in a Teflon cylinder attached to a copper bottom plate cooled at $-25^{\circ}C$. Improved dispersion stability of camphene slurry and the homogeneous frozen body was achieved using the oxidized Sn powder at $670^{\circ}C$ in air after ball milling. The porous Sn specimen, prepared by freeze-drying of the camphene slurry with oxidized Sn powder from the heat-treated Sn/tin chloride mixture and sintering at $1100^{\circ}C$ for 1 h in a hydrogen atmosphere, showed large pores of about $200{\mu}m$, which were aligned parallel to the camphene growth direction, and small pores in their internal walls. However, $100{\mu}m$ spherical particles were observed in the bottom part of the specimen due to the melting of the Sn powder during sintering of the green compact.