• Journal of Powder Materials
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• v.21 no.3
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• pp.191-195
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• 2014

This study reports a simple way of fabricating the porous Cu with unidirectional pore channels by freeze drying camphene slurry with Cu oxide coated Cu powders. The coated powders were prepared by calcination of ball-milled powder mixture of Cu and Cu-nitrate. Improved dispersion stability of camphene slurry could be achieved using the Cu oxide coated Cu powders instead of pure Cu powders. Pores in the frozen specimen at $-25^{\circ}C$ were generated by sublimation of the camphene during drying in air, and the green bodies were sintered at $750^{\circ}C$ for 1 h in $H_2$ atmosphere. XRD analysis revealed that the coated layer of Cu oxide was completely converted to Cu phase without any reaction phases by hydrogen heat treatment. The porous Cu specimen prepared from pure Cu powders showed partly large pores with unidirectional pore channels, but most of pores were randomly distributed. In contrast, large and aligned parallel pores to the camphene growth direction were clearly observed in the sample using Cu oxide coated Cu powders. Pore formation behavior depending on the initial powders was discussed based on the degree of powder rearrangement and dispersion stability in slurry.

• Journal of Powder Materials
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• v.23 no.1
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• pp.49-53
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• 2016

The present study demonstrates the effect of freezing conditions on the pore structure of porous Cu-10 wt.% Sn prepared by freeze drying of $CuO-SnO_2$/camphene slurry. Mixtures of CuO and $SnO_2$ powders are prepared by ball milling for 10 h. Camphene slurries with 10 vol.% of $CuO-SnO_2$ are unidirectionally frozen in a mold maintained at a temperature of $-30^{\circ}C$ for 1 and 24 h, respectively. Pores are generated by the sublimation of camphene at room temperature. After hydrogen reduction and sintering at $650^{\circ}C$ for 2 h, the green body of the $CuO-SnO_2$ 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 $300{\mu}m$ 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.

• Korean Journal of Materials Research
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• v.23 no.12
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• pp.722-726
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• 2013

Freeze drying of a porous Cu-Sn alloy with unidirectionally aligned pore channels was accomplished by using a composite powder of CuO-$SnO_2$ and camphene. Camphene slurries with CuO-$SnO_2$ content of 3, 5 and 10 vol% were prepared by mixing with a small amount of dispersant at $50^{\circ}C$. Freezing of a slurry was done 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 bodies were hydrogen-reduced at $650^{\circ}C$ and then were sintered at $650^{\circ}C$ and $750^{\circ}C$ for 1 h. XRD analysis revealed that the CuO-$SnO_2$ powder was completely converted to Cu-Sn alloy without any reaction phases. The sintered samples showed large pores with an average size of above $100{\mu}m$ which were aligned parallel to the camphene growth direction. Also, the internal walls of the large pores had relatively small pores. The size of the large pores decreased with increasing CuO-$SnO_2$ content due to the change of the degree of powder rearrangement in the slurry. The size of the small pores decreased with increase of the sintering temperature from $650^{\circ}C$ to $750^{\circ}C$, while that of the large pores was unchanged. These results suggest that a porous alloy body with aligned large pores can be fabricated by a freeze-drying and hydrogen reduction process using oxide powders.

• Korean Journal of Materials Research
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• v.23 no.1
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• pp.67-71
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• 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.

• Journal of Powder Materials
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• v.28 no.3
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• pp.216-220
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• 2021

The effect of tert-butyl alcohol (TBA) as a freezing solvent on the pore structure of a porous tungsten body prepared by freeze-drying is analyzed. TBA slurries with a WO3 content of 10 vol% are prepared by mixing with a small amount of dispersant and binder at 30℃. The slurries are frozen at -25℃, and pores are formed in the frozen specimens by the sublimation of TBA during drying in air. After hydrogen reduction at 800℃ and sintering at 1000℃, the green body of WO₃ is completely converted to porous W with various pore structures. Directional pores from the center of the specimen to the outside are observed in the sintered bodies because of the columnar growth of TBA. A decrease in pore directionality and porosity is observed in the specimens prepared by long-duration drying and sintering. The change in pore structure is explained by the growth of the freezing solvent and densification.

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

• Journal of Powder Materials
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• v.24 no.6
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• pp.472-476
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• 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.

• Korean Journal of Materials Research
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• v.28 no.2
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• pp.108-112
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• 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.

• Journal of Powder Materials
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• v.25 no.1
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• pp.25-29
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• 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.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2010.06a
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• pp.375-375
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• 2010

CdTe as an absorber material is widely used in thin film solar cells with the heterostructure due to its almost ideal band gap energy of 1.45 eV, high photovoltaic conversion efficiency, low cost and stable performance. The deposition methods and preparation conditions for the fabrication of CdTe are very important for the achievement of high solar cell conversion efficiency. There are some rearranged reports about the deposition methods available for the preparation of CdTe thin films such as close spaced sublimation (CSS), physical vapor deposition (PVD), vacuum evaporation, vapor transport deposition (VTD), closed space vapor transport, electrodeposition, screen printing, spray pyrolysis, metalorganic chemical vapor deposition (MOCVD), and RF sputtering. The RF sputtering method for the preparation of CdTe thin films has important advantages in that the thin films can be prepared at low growth temperatures with large-area deposition suitable for mass-production. The authors reported that the optical and electrical properties of CdTe thin film were closely connected by the thickness-uniformity of the film in the previous study [1], which means that the better optical absorbance and the higher carrier concentration could be obtained in the better condition of thickness-uniformity for CdTe thin film. The thickness-uniformity could be controlled and improved by the some process parameters such as vacuum level and RF power in the sputtering process of CdTe thin films. However, there is a limitation to improve the thickness-uniformity only in the preparation process [1]. So it is necessary to introduce the external or additional method for improving the thickness-uniformity of CdTe thin film because the cell size of thin film solar cell will be enlarged. Therefore, the authors firstly applied the chemical mechanical polishing (CMP) process to improving the thickness-uniformity of CdTe thin films with a G&P POLI-450 CMP polisher [2]. CMP process is the most important process in semiconductor manufacturing processes in order to planarize the surface of the wafer even over 300 mm and to form the copper interconnects with damascene process. Some important CMP characteristics for CdTe were obtained including removal rate (RR), WIWNU%, RMS roughness, and peak-to-valley roughness [2]. With these important results, the CMP process for CdTe thin films was performed to improve the thickness-uniformity of the sputtering-deposited CdTe thin film which had the worst two thickness-uniformities of them. Some optical properties including optical transmittance and absorbance of the CdTe thin films were measured by using a UV-Visible spectrophotometer (Varian Techtron, Cary500scan) in the range of 400 - 800 nm. After CMP process, the thickness-uniformities became better than that of the best condition in the previous sputtering process of CdTe thin films. Consequently, the optical properties were directly affected by the thickness-uniformity of CdTe thin film. The absorbance of CdTe thin films was improved although the thickness of CdTe thin film was not changed.