• Journal of Powder Materials
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• v.25 no.4
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• pp.336-339
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• 2018

A unique porous material with controlled pore characteristics can be fabricated by the freeze-drying process, which uses the slurry of organic material as the sublimable vehicle mixed with powders. The essential feature in this process is that during the solidification of the slurry, the dendrites of the organic material should repel the dispersed particles into the interdendritic region. In the present work, a model experiment is attempted using some transparent organic materials mixed with glass powders, which enable in-situ observation. The organic materials used are camphor-naphthalene mixture (hypo- and hypereutectic composition), salol, camphene, and pivalic acid. Among these materials, the constituent phases in camphor-naphthalene system, i.e. naphthalene plate, camphor dendrite, and camphor-naphthalene eutectic exclusively repel the glass powders. This result suggests that the control of organic material composition in the binary system is useful for producing a porous body with the required pore structure.

• Journal of Powder Materials
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• v.20 no.4
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• pp.253-257
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• 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
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• v.22 no.5
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• pp.362-366
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• 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
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• v.27 no.3
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• pp.198-202
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• 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.