• Transactions of the Korean hydrogen and new energy society
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• v.29 no.5
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• pp.434-441
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• 2018

The pore size of nickel (Ni) bottom electrode layer (BEL) for low-temperature solid oxide fuel cells embedded with ultrathin-film electrolyte was controlled by changing the substrate surface morphology and deposition process parameters. For ~150-nm-thick Ni BEL, the upper side of an anodic aluminum oxide (AAO) substrate with ~65-nm-sized pores provided ~1.7 times smaller pore size than the lower side of the AAO substrate. For ~100-nm-thick Ni BEL, the AAO substrate with ~45-nm-sized pores provided ~2.6 times smaller pore size than the AAO substrate with ~95-nm-sized pores, and the deposition pressure of ~4 mTorr provided ~1.3 times smaller pore size than that of ~48 mTorr. On the AAO substrate with ~65-nm-sized pores, the Ni BEL deposited for 400 seconds had ~2 times smaller pore size than the Ni BEL deposited for 100 seconds.

• Korean Journal of Materials Research
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• v.25 no.11
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• pp.602-606
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• 2015

Porous W with spherical and directionally aligned pores was fabricated by the combination of sacrificial fugitives and a freeze-drying process. Camphene slurries with powder mixtures of $WO_3$ and spherical PMMA of 20 vol% were frozen at $-25^{\circ}C$ and dried for the sublimation of the camphene. The green bodies were heat-treated at $400^{\circ}C$ for 2 h to decompose the PMMA; then, sintering was carried out at $1200^{\circ}C$ in a hydrogen atmosphere for 2 h. TGA and XRD analysis showed that the PMMA decomposed at about $400^{\circ}C$, and $WO_3$ was reduced to metallic W at $800^{\circ}C$ without any reaction phases. The sintered bodies with $WO_3$-PMMA contents of 15 and 20 vol% showed large pores with aligned direction and small pores in the internal walls of the large pores. The pore formation was discussed in terms of the solidication behavior of liquid camphene with solid particles. Spherical pores, formed by decomposition of PMMA, were observed in the sintered specimens. Also, microstructural observation revealed that struts between the small pores consisted of very fine particles with size of about 300 nm.

• 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.

• 한국신재생에너지학회:학술대회논문집
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• 2006.06a
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• pp.9-12
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• 2006

We performed molecular dynamics simulations on the conventional MOF, IRMOF-14 and the catenated MOF with two MOF chains, IRMOF13, to find out rational design and synthetic strategies toward efficient hydrogen storage materials. The molecular dynamics calculations were done using Universal force fields and the analysis of result was performed during the NVE dynamics after preliminary NVT dynamics at 77K. The results showed the density of adsorbed hydrogen molecules was increased in the various pores created by catenation of MOFs while the large amount of volume in conventional MOF was not effectively utilized to store hydrogen. Those calculation results commonly showed the proper control of pore si Be for hydrogen storage into MOF by catenation would be one of the efficient ways to increase hydrogen capacity of MOFs.

• Journal of Powder Materials
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• v.18 no.4
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• pp.327-331
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• 2011

In order to fabricate the porous metal with controlled pore characteristics, unique processing by using metal oxide powder as the source and camphene as the sublimable material is introduced. CuO powder was selected as the source for the formation of Cu metal via hydrogen reduction. Camphene-based CuO slurry, prepared by milling at $47^{\circ}C$ with a small amount of dispersant, was frozen at $-25^{\circ}C$. Pores were generated subsequently by sublimation of the camphene. The green body was hydrogen-reduced at $200^{\circ}C$ for 30 min, and sintered at $500-700^{\circ}C$ for 1 h. Microstructural analysis revealed that the sintered Cu showed aligned large pore channels parallel to the camphene growth direction, and fine pores are formed around the large pore. Also, it showed that the pore size was controllable by the slurry concentration.

• Korean Journal of Metals and Materials
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• v.47 no.9
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• pp.597-603
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• 2009

The hydrogen reduction behavior of ultrasonic ball-milled $WO_3-CuO$ nanopowder, which is highly related with micro-pore structure, was investigated by thermogravimetry(TG) and hygrometry system. EDS and TEM results represented that the ultrasonic ball-milled $WO_3-CuO$ nanopowder consisted of the agglomerates which was confirmed as a homogeneous mixture of $WO_3$ and CuO particles. It was found that the reduction reaction of CuO was retarded by initial micro-pores which are smaller than 40 nm in the ultrasonic ball-milled $WO_3-CuO$ nanopowder. The earlier agglomeration of Cu particles at comparably low temperature decreased the volume of micro-pores in the $WO_3-CuO$ nanopowder which caused the retardation of $WO_3$ reduction reaction. These results clearly explain that the micro-pore structure significantly affected the reduction reaction of $WO_3$ and CuO in the $WO_3-CuO$ nanopowder.

• 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.

• 한국신재생에너지학회:학술대회논문집
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• 2009.06a
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• pp.744-744
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• 2009

The development of safe and suitable hydrogen storage materials is one of key issues for commercializing hydrogen as an energy carrier. Carbon based materials have been investigated for many years to store hydrogen by the adsorption of the gas on the surface of the carbon structure. Recently, it is reported that carbon nitride nanobells have high hydrogen storage capacity since the nitrogen atom plays an important role on attracting hydrogen molecules. Here we report carbon nitride microporous spheres (CNMS) which have the maximum surface area of 995.3 $m^2/g$. Melamine-Formaldehyde resin is the source of carbon and nitrogen in CNMS. Most of the CNMS pores have diameters in the range of 6 to 8 A which could give a penetration energy barrier to a certain molecule. In addition, the maximum hydrogen storage capacities of carbon nitride spheres are 1.9 wt% under 77 K and 1 atm.

• 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.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.