Tert-butyl alcohol의 동결주조에 의한 방향성 기공 함유 TiO₂ 다공체 제조

The effect of freezing conditions on the pore structure of porous TiO₂ fabricated using a freeze casting process with tert-butyl alcohol slurry was investigated. The raw powder was heat treated to manufacture a porous body with stable shape by suppressing volume change induced by the phase transformation of TiO₂ powder. The XRD analysis result indicated that the anatase phase fraction in the raw powder could be converted to 98.6% rutile phase by heating it at 800°C for 30 min. Porous TiO₂ ceramics with unidirectionally aligned pore channels were prepared by freezing tert-butyl alcohol slurry containing 10 vol% TiO₂ powder under different freezing temperatures of -20, -30 and -40°C, respectively. After removing the frozen tert-butyl alcohol by sublimation in vacuum, the green samples were sintered at 1100°C for 4 h in air. The porous body contains directional pores with a size of approximately 30 µm, and a hexagonal pore shape corresponding to the crystal structure of tert-butyl alcohol was observed in the cross-section of the pores. Small pores were observed at the bottom part of the porous body near the Cu plate where the solidification heat was released, but relatively large pores were present at the upper part. Both microstructure observation and pore size distribution indicated that the pore size and the strut thickness increased significantly with increasing freezing temperature. The change in pore characteristics was explained as being mainly due to the difference in the solidification behavior of the slurry and the rearrangement of the solid powder.