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°C. Freezing of a slurry is performed at -25°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°C and then sintered at 800°C and 900°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.
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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-SnO2/camphene slurry. Mixtures of CuO and SnO2 powders are prepared by ball milling for 10 h. Camphene slurries with 10 vol.% of CuO-SnO2 are unidirectionally frozen in a mold maintained at a temperature of -30°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°C for 2 h, the green body of the CuO-SnO2 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 μm 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.
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In order to fabricate the porous Al2O3 with dispersion of nano-sized Cu particles, freeze-drying of camphene/ Al2O3 slurry and solution chemistry process using Cu-nitrate are introduced. Camphene slurries with 10 vol% Al2O3 was frozen at -25°C. Pores were generated by sublimation of the camphene during drying in air. The sintered samples at 1400 and 1500°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 Al2O3/1 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.
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