• 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.

• Journal of Powder Materials
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• v.26 no.1
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• pp.40-44
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• 2019

Tungsten trioxide ($WO_3$) is a promising candidate as a photocatalyst because of its outstanding electrical and optical properties. In this study, we prepare $WO_3$ thin films by electrodeposition and characterize the photocatalytic degradation of methylene blue using these films. Depending on the voltage conditions (static and pulse), compact and porous $WO_3$ films are fabricated on a transparent ITO/glass substrate. The morphology and crystal structure of electrodeposited $WO_3$ thin films are investigated by scanning electron microscopy, atomic force microscopy, and X-ray diffraction. An application of static voltage during electrodeposition yields a compact layer of $WO_3$, whereas a highly porous morphology with nanoflakes is produced by a pulse voltage process. Compared to the compact film, the porous $WO_3$ thin film shows better photocatalytic activities. Furthermore, a much higher reaction rate of degradation of methylene blue can be achieved after post-annealing of $WO_3$ thin films.

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.10a
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• pp.16.1-16.1
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• 2011

Gas sensor properties of $WO_3$ nanowire structures have been studied. The sensing layer was prepared by deposition of tungsten metal on porous single wall carbon nanotubes followed by thermal oxidation. The morphology and crystalline quality of $WO_3$ material was investigated by SEM, TEM, XRD and Raman analysis. A highly porous $WO_3$ nanowire structure with a mean diameter of 82 nm was obtained. Response to CO, $NH_3$ and $H_2$ gases diluted in air were investigated in the temperature range of $100{\sim}340^{\circ}C$ The sensor exhibited low response to CO gas and quite high response to $NH_3$ and $H_2$ gases. The highest sensitivity was observed at $250^{\circ}C$ for $NH_3$ and $300^{\circ}C$ for $H_2$. The effect of the diameters of $WO_3$ nanowires on the sensor performance was also studied. The $WO_3$ nanowires sensor with diameter of 40 nm showed quite high sensitivity, fast response and recovery times to $H_2$ diluted in dry air. The sensitivity as a function of detecting gas concentrations and gas sensing mechanism was discussed. The effect of dilution carrier gases, dry air and nitrogen, was examined.

• Journal of Powder Materials
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• v.22 no.2
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• pp.129-133
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• 2015

Porous W with controlled pore structure was fabricated by thermal decomposition and hydrogen reduction process of PMMA beads and $WO_3$ powder compacts. The PMMA sizes of 8 and $50{\mu}m$ were used as pore forming agent for fabricating the porous W. The $WO_3$ powder compacts with 20 and 70 vol% PMMA were prepared by uniaxial pressing and sintered for 2 h at $1200^{\circ}C$ in hydrogen atmosphere. TGA analysis revealed that the PMMA was decomposed at about $400^{\circ}C$ and $WO_3$ was reduced to metallic W at $800^{\circ}C$. Large pores in the sintered specimens were formed by thermal decomposition of spherical PMMA, and their size was increased with increase in PMMA size and the amount of PMMA addition. Also the pore shape was changed from spherical to irregular form with increasing PMMA contents due to the agglomeration of PMMA in the powder mixing process.

• Journal of Sensor Science and Technology
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• v.27 no.5
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• pp.345-351
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• 2018

We employed an unprecedented technique to synthesize porous $WO_3@SnO_2$ nanofibers exhibiting core-shell and fiber-in-tube configurations. Firstly, 2-methylimidazole was uniformly incorporated in as-spun nanofibers containing ammonium metatungstate hydrate and the sacrificial polymer (polyacrylonitrile). Secondly, the 2-methylimidazole on the surfaces of nanofibers was complexed with tin(II) chloride ($SnCl_2$) via simple impregnation of the as-spun nanofibers in ethanol containing tin(II) chloride dihydrate ($SnCl_2{\cdot}2H_2O$). The presence of vacant p-orbitals in tin (Sn) and the nucleophilic nitrogen on the imidazole ring allowed for the reaction between $SnCl_2$ and 2-methylimidazole, forming adducts on the surfaces of the as-spun nanofibers. The calcination of these nanofibers resulted in porous $WO_3@SnO_2$ nanofibers with a higher surface area ($55.3m^2{\cdot}g^{-1}$) and a better response to 1-5 ppm of acetone than pristine $SnO_2$ NFs synthesized using a similar method. An improved response to acetone was achieved upon functionalization of the $WO_3@SnO_2$ nanofibers with catalytic palladium nanoparticles. This work demonstrates the potential application of $WO_3@SnO_2$ nanofibers as sensing layers for chemiresistive sensory devices for the detection of acetone in exhaled breath.

• 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.29 no.2
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• pp.118-122
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• 2022

The synthesis of porous W by freeze-casting and vacuum drying is investigated. Ball-milled WO₃ powders and tert-butyl alcohol were used as the starting materials. The tert-butyl alcohol slurry is frozen at -25℃ and dried under vacuum at -25 and -10℃. The dried bodies are hydrogen-reduced at 800℃ and sintered at 1000℃. The XRD analysis shows that WO₃ is completely reduced to W without any reaction phases. SEM observations reveal that the struts and pores aligned in the tert-butyl alcohol growth direction, and the change in the powder content and drying temperature affects the pore structure. Furthermore, the struts of the porous body fabricated under vacuum are thinner than those fabricated under atmospheric pressure. This behavior is explained by the growth mechanism of tert-butyl alcohol and rearrangement of the powders during solidification. These results suggest that the pore structure of a porous body can be controlled by the powder content, drying temperature, and pressure.

• 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.28 no.4
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• pp.331-335
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• 2021

The effects of drying temperature on the microstructure of porous W fabricated by the freeze-casting process of tert-butyl alcohol slurry with WO₃ powder was investigated. Green bodies were hydrogen-reduced at 800℃ for 1 h and sintered at 1000℃ for 6 h. X-ray diffraction analysis revealed that WO₃ powders were completely converted to W without any reaction phases by hydrogen reduction. The sintered body showed pores aligned in the direction of tert-butyl alcohol growth, and the porosity and pore size decreased as the amount of WO₃ increased from 5 to 10vol%. As the drying temperature of the frozen body increased from -25℃ to -10℃, the pore size and thickness of the struts increased. The change in microstructural characteristics based on the amount of powder added and the drying temperature was explained by the growth behavior of the freezing agent and the degree of rearrangement of the solid powder during the solidification of the slurry.

• Journal of Powder Materials
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• v.19 no.4
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• pp.259-263
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• 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.