• Journal of Powder Materials
• /
• v.21 no.5
• /
• pp.366-370
• /
• 2014

The present study demonstrates the effect of solidification condition on the pore structure in freeze drying process using the slurries of CuO/sublimable vehicles. Camphene and Camphor-45 wt% naphthalene based slurries with 14 vol% CuO powder were frozen into a mold at $-25^{\circ}C$, followed by sublimation at room temperature. The green bodies were hydrogen-reduced and sintered at $500^{\circ}C$ for 1 h. The porous Cu specimen, frozen the CuO/camphene slurry into the heated mold of the upper part, showed large pores with unidirectional pore channels and small pores in their internal wall. Also, it was observed that the size of large pores was decreasing near the bottom part of specimen. The change of pore structure depending on the freezing condition was explained by the nucleation behavior of camphene crystals and rearrangement of solid powders during solidification. In case of porous Cu prepared from CuO/Camphor-naphthalene system, the pore structure exhibited plate shape as a replica of the original structure of crystallized vehicles with hypereutectic composition.

• Journal of Powder Materials
• /
• v.27 no.3
• /
• pp.198-202
• /
• 2020

The effect of sublimable vehicles on the pore structure of Cu fabricated by freeze drying is investigated. The 5 vol% CuO-dispersed slurries with camphene and various camphor-naphthalene compositions are frozen in a Teflon mold at -25℃, followed by sublimation at room temperature. After hydrogen reduction at 300℃ and sintering at 600 ℃, the green bodies of CuO are completely converted to Cu with various pore structures. The sintered samples prepared using CuO/camphene slurries show large pores that are aligned parallel to the sublimable vehicle growth direction. In addition, a dense microstructure is observed in the bottom section of the specimen where the solidification heat was released, owing to the difference in the solidification behavior of the camphene crystals. The porous Cu shows different pore structures, such as dendritic, rod-like, and plate shaped, depending on the composition of the camphornaphthalene system. The change in pore structure is explained by the crystal growth behavior of primary camphor and eutectic and primary naphthalene.

• Journal of Powder Materials
• /
• v.22 no.5
• /
• pp.362-366
• /
• 2015

The effect of sublimable vehicle composition in the camphor-naphthalene system on the pore structure of porous Cu-Ni alloy is investigated. The CuO-NiO mixed slurries with hypoeutectic, eutectic and hypereutectic compositions are frozen into a mold at $-25^{\circ}C$. Pores are generated by sublimation of the vehicles at room temperature. After hydrogen reduction at $300^{\circ}C$ and sintering at $850^{\circ}C$ for 1 h, the green body of CuO-NiO is completely converted to porous Cu-Ni alloy with various pore structures. The sintered samples show large pores which are aligned parallel to the sublimable vehicle growth direction. The pore size and porosity decrease with increase in powder content due to the degree of powder rearrangement in slurry. In the hypoeutectic composition slurry, small pores with dendritic morphology are observed in the sintered Cu-Ni, whereas the specimen of hypereutectic composition shows pore structure of plate shape. The change of pore structure is explained by growth behavior of primary camphor and naphthalene crystals during solidification of camphor-naphthalene alloys.

• Journal of Powder Materials
• /
• v.20 no.4
• /
• pp.253-257
• /
• 2013

Freeze drying for porous Mo was accomplished by using $MoO_3$ powder as the source and camphor-naphthalene eutectic system as the sublimable material. Eutectic composition of camphor-naphthalene slurries with the initial $MoO_3$ content of 5 vol%, prepared by milling at $55^{\circ}C$ with a small amount of oligomeric dispersant, was frozen at $-25^{\circ}C$. The addition of dispersant showed improvement of dispersion stability in slurries. Pores were generated subsequently by sublimation of the camphor-naphthalene during drying in air for 48 h. To convert the $MoO_3$ to metallic Mo, the green body was hydrogen-reduced at $750^{\circ}C$, and sintered at $1100^{\circ}C$ for 2 h. The sintered samples, frozen by heated Teflon cylinder, showed large pores with the size of about 40 ${\mu}m$ which were aligned parallel to the sublimable vehicles growth direction. The formation of unidirectionally aligned pores is explained by the rejection and accumulation of solid particles in the serrated solid-liquid interface.

• Journal of Powder Materials
• /
• v.21 no.1
• /
• pp.16-20
• /
• 2014

In order to fabricate the porous $Al_2O_3$ with dispersion of nano-sized Cu particles, freeze-drying of camphene/$Al_2O_3$ slurry and solution chemistry process using Cu-nitrate are introduced. Camphene slurries with 10 vol% $Al_2O_3$ was frozen at $-25^{\circ}C$. Pores were generated by sublimation of the camphene during drying in air. The sintered samples at 1400 and $1500^{\circ}C$ showed the same size of large pores which were aligned parallel to the sublimable vehicles growth direction. However, the size of fine pores in the internal walls of large pores decreased with increase in sintering temperature. It was shown that Cu particles with the size of 100 nm were homogeneously dispersed on the surfaces of the large pores. Antibacterial test using fungus revealed that the porous $Al_2O_3$/1 vol% Cu composite showed antifungal property due to the dispersion of Cu particles. The results are suggested that the porous composites with required pore characteristics and functional property can be fabricated by freeze-drying process and addition of functional nano particles by chemical method.

• Korean Journal of Materials Research
• /
• v.21 no.9
• /
• pp.520-524
• /
• 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
• /
• v.23 no.6
• /
• pp.339-343
• /
• 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.