• 한국분말재료학회지
• /
• 제19권4호
• /
• pp.259-263
• /
• 2012

Dependence of the freeze-drying process condition on microstructure of porous W and pore formation mechanism were studied. Camphene slurries with $WO_3$ contents of 10 vol% were prepared by milling at $50^{\circ}C$ with a small amount of dispersant. Freezing of a slurry was done in Teflon cylinder attached to a copper bottom plate cooled 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 $800^{\circ}C$ for 30 min, and sintered in the furnace at $900^{\circ}C$ for 1 h. After heat treatment in hydrogen atmosphere, $WO_3$ powders were completely converted to metallic W without any reaction phases. The sintered samples showed large pores with the size of about $70{\mu}m$ 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 with dendritic structure due to the growth of camphene dendrite depending on the degree of nucleation and powder rearrangement in the slurry.

• 한국분말재료학회지
• /
• 제27권3호
• /
• pp.193-197
• /
• 2020

Porous Cu-14 wt% Co with aligned pores is produced by a freeze drying and sintering process. Unidirectional freezing of camphene slurry with CuO-Co₃O₄ powders is conducted, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The dried bodies are hydrogen-reduced at 500℃ and sintered at 800℃ for 1 h. The reduction behavior of the CuO-Co₃O₄ powder mixture is analyzed using a temperature-programmed reduction method in an Ar-10% H₂ atmosphere. The sintered bodies show large and aligned parallel pores in the camphene growth direction. In addition, small pores are distributed around the internal walls of the large pores. The size and fraction of the pores decrease as the amount of solid powder added to the slurry increases. The change in pore characteristics according to the amount of the mixed powder is interpreted to be due to the rearrangement and accumulation behavior of the solid particles in the freezing process of the slurry.

• 한국재료학회지
• /
• 제26권2호
• /
• pp.61-66
• /
• 2016

In order to fabricate porous mullite ceramics with controlled pore structure and improved mechanical strength, a freeze casting route has been processed using camphene mixed with tertiary-butyl alcohol (TBA) and coal fly ash/alumina as the solvent and the ceramic material, respectively. After sintering, the solidification characteristics of camphene and TBA solvent were evident in the pore morphology, i.e., dendritic and straight pore channels formed along the solidification directions of camphene and TBA ice, respectively, after sublimation. Also, the presence of microcracks was observed in the bodies sintered at $1500^{\circ}C$, mainly due to the difference in solidification volume change between camphene and TBA. The compressive strength of the sintered bodies was found generally to be dependent, in an inverse manner, on the porosity, which was mainly determined by the processing conditions. After sintering at $1300{\sim}1500^{\circ}C$ with 30~50 wt% solid loading, the resulting mullite ceramics showed porosity and compressive strength values in ranges of 83.8~43.1% and 3.7~206.8 MPa, respectively.

• 한국분말재료학회지
• /
• 제22권2호
• /
• pp.122-128
• /
• 2015

In this study, titanium(Ti) meshes and porous bodies are employed to synthesize carbon nanotubes(CNTs) using methane($CH_4$) gas and camphene solution, respectively, by chemical vapor deposition. Camphene is impregnated into Ti porous bodies prior to heating in a furnace. Various microscopic and spectroscopic techniques are utilized to analyze CNTs. It is found that CNTs are more densely and homogeneously populated on the camphene impregnated Ti-porous bodies as compared to CNTs synthesized with methane on Ti-porous bodies. It is elucidated that, when synthesized with methane, few CNTs are formed inside of Ti porous bodies due to methane supply limited by internal structures of Ti porous bodies. Ti-meshes and porous bodies are found to be multi-walled with high degree of structural disorders. These CNTs are expected to be utilized as catalyst supports in catalytic filters and purification systems.

• 한국재료학회지
• /
• 제28권2호
• /
• pp.108-112
• /
• 2018

The present study demonstrates the effect of raw powder on the pore structure of porous W-Ni prepared by freeze drying of camphene-based slurries and sintering process. The reduction behavior of $WO_3$ and $WO_3-NiO$ powders is analyzed by a temperature programmed reduction method in Ar-10% H2 atmosphere. After heat treatment in hydrogen atmosphere, $WO_3-NiO$ powder mixture is completely converted to metallic W without any reaction phases. Camphene slurries with oxide powders are frozen at $-30^{\circ}C$, and pores in the frozen specimens are generated by sublimation of the camphene during drying in air. The green bodies are hydrogen-reduced at $800^{\circ}C$ and sintered at $1000^{\circ}C$ for 1 h. The sintered samples show large and aligned parallel pores to the camphene growth direction, and small pores in the internal wall of large pores. The strut between large pores, prepared from pure $WO_3$ powder, consists of very fine particles with partially necking between the particles. In contrast, the strut densification is clearly observed in the Ni-added W sample due to the enhanced mass transport in activation sintering.

• 한국재료학회지
• /
• 제23권1호
• /
• pp.67-71
• /
• 2013

Porous $Al_2O_3$ dispersed with nano-sized Cu was fabricated by freeze-drying process and solution chemistry method using Cu-nitrate. To prepare porous $Al_2O_3$, camphene was used as the sublimable vehicle. Camphene slurries with $Al_2O_3$ content of 10 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 to $-25^{\circ}C$ while unidirectionally controlling the growth direction of the camphene. Pores were subsequently generated by sublimation of the camphene during drying in air for 48 h. The green body was sintered in a furnace at $1400^{\circ}C$ for 1 h. Cu particles were dispersed in porous $Al_2O_3$ by calcination and hydrogen reduction of Cu-nitrate. The sintered samples showed large pores with sizes of about $150{\mu}m$; these pores were aligned parallel to the camphene growth direction. Also, the internal walls of the large pores had relatively small pores due to the traces of camphene left between the concentrated $Al_2O_3$ particles on the internal wall. EDS analysis revealed that the Cu particles were mainly dispersed on the surfaces of the large pores. These results strongly suggest that porous $Al_2O_3$ with Cu dispersion can be successfully fabricated by freeze-drying and solution chemistry routes.

• 한국분말재료학회지
• /
• 제25권1호
• /
• pp.25-29
• /
• 2018

Porous Cu with a dispersion of nanoscale $Al_2O_3$ particles is fabricated by freeze-drying $CuO-Al_2O_3$/camphene slurry and sintering. Camphene slurries with $CuO-Al_2O_3$ contents of 5 and 10 vol% are unidirectionally frozen at $-30^{\circ}C$, and pores are generated in the frozen specimens by camphene sublimation during air drying. The green bodies are sintered for 1 h at $700^{\circ}C$ and $800^{\circ}C$ in $H_2$ atmosphere. The sintered samples show large pores of $100{\mu}m$ in average size aligned parallel to the camphene growth direction. The internal walls of the large pores feature relatively small pores of ${\sim}10{\mu}m$ in size. The size of the large pores decreases with increasing $CuO-Al_2O_3$ content by the changing degree of powder rearrangement in the slurry. The size of the small pores decreases with increasing sintering temperature. Microstructural analysis reveals that 100-nm $Al_2O_3$ particles are homogeneously dispersed in the Cu matrix. These results suggest that a porous composite body with aligned large pores could be fabricated by a freeze-drying and $H_2$ reducing process.

• 한국분말재료학회지
• /
• 제26권1호
• /
• pp.1-5
• /
• 2019

In this study, porous Mo-5 wt% Cu with unidirectionally aligned pores is prepared by freeze drying of camphene slurry with $MoO_3-CuO$ powders. Unidirectional freezing of camphene slurry with dispersion stability is conducted at $-25^{\circ}C$, and pores in the frozen specimens are generated by sublimation of the camphene crystals. The green bodies are hydrogen-reduced at $750^{\circ}C$ and sintered at $1000^{\circ}C$ for 1 h. X-ray diffraction analysis reveals that $MoO_3-CuO$ composite powders are completely converted to a Mo-and-Cu phase without any reaction phases by hydrogen reduction. The sintered bodies with the Mo-Cu phase show large and aligned parallel pores to the camphene growth direction as well as small pores in the internal walls of large pores. The pore size and porosity decrease with increasing composite powder content from 5 to 10 vol%. The change of pore characteristics is explained by the degree of powder rearrangement in slurry and the accumulation behavior of powders in the interdendritic spaces of solidified camphene.

• 원예과학기술지
• /
• 제28권4호
• /
• pp.696-700
• /
• 2010

국내외에서 유통되고 있는 로즈마리 정유 31점을 수집하여 GC통한 유효성분분석과 항산화 활력시험을 실시하였다. 주요 성분은 ${\alpha}$-pinene, camphene, ${\beta}$-pinene, 1.8-cineol, verbenone 및 borneol 등이 동정되었다. 주요성분에 따라 생산국별로 함량의 차이가 나타났으며, 프랑스 원산 정유의 품질이 우수하였고, 국내에서 재배하여 추출한 정유가 ${\alpha}$-pinene과 camphene의 함량이 높았다. ISO가 제시한 9가지 성분의 함량을 충족하는 제품은 총 31점 중 5점(16%)으로 낮았다. 전자공여능(EDA)은 4.8-96.0%로 현저한 차이를 보였으며, 60%이상의 항산화능 활력을 갖는 정유는 13%였다. 특정 성분 함량에 따른 항산화 활력정도의 차이는 일치하지 않았으며, 스위스 원산의 정유에서 가장 높은 항산화 활력을 보였다.

• 한국분말재료학회지
• /
• 제24권6호
• /
• pp.472-476
• /
• 2017

Porous W-10 wt% Ti alloys are prepared by freeze-drying a $WO_3-TiH_2$/camphene slurry, using a sintering process. X-ray diffraction analysis of the heat-treated powder in an argon atmosphere shows the $WO_3$ peak of the starting powder and reaction-phase peaks such as $WO_{2.9}$, $WO_2$, and $TiO_2$ peaks. In contrast, a powder mixture heated in a hydrogen atmosphere is composed of the W and TiW phases. The formation of reaction phases that are dependent on the atmosphere is explained by a thermodynamic consideration of the reduction behavior of $WO_3$ and the dehydrogenation reaction of $TiH_2$. To fabricate a porous W-Ti alloy, the camphene slurry is frozen at $-30^{\circ}C$, and pores are generated in the frozen specimens by the sublimation of camphene while drying in air. The green body is hydrogen-reduced and sintered at $1000^{\circ}C$ for 1 h. The sintered sample prepared by freeze-drying the camphene slurry shows large and aligned parallel pores in the camphene growth direction, and small pores in the internal walls of the large pores. The strut between large pores consists of very fine particles with partial necking between them.