• 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.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.6
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• pp.245-250
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• 2019

We investigated the post-annealing effect of Sn-incorporated β-Ga₂O₃ (β-Ga₂O₃ : Sn) nanowires (NWs) grown on sapphire (0001) substrates using radio-frequency powder sputtering. The β-Ga₂O₃ : Sn NWs were converted to a porous structure during the vacuum annealing process at 800℃. Host non-stoichiometric Ga₂O_3-x, is transformed into stoichiometric Ga₂O₃, where Sn atoms separate and form Sn nano-clusters that gradually evaporate in a vacuum atmosphere. As a result, the amount of Sn atoms was reduced from 1.31 to 0.27 at%. Pores formed on the sides of β-Ga₂O₃ : Sn NWs were observed. This increases the ratio of the surface to the volume of β-Ga₂O₃ : Sn NWs.

• Journal of Powder Materials
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• v.31 no.2
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• pp.146-151
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• 2024

Pure SnO₂ has proven very difficult to densify. This poor densification can be useful for the fabrication of SnO₂ with a porous microstructure, which is used in electronic devices such as gas sensors. Most electronic devices based on SnO₂ have a porous microstructure, with a porosity of > 40%. In pure SnO₂, a high sintering temperature of approximately 1300℃ is required to obtain > 40% porosity. In an attempt to reduce the required sintering temperature, the present study investigated the low-temperature sinterability of a current system. With the addition of TiO₂, the compositions of the samples were Sn_1-xTi_xO₂-CoO(0.3wt%)-CuO(2wt%) in the range of x ≤ 0.04. Compared to the samples without added TiO₂, densification was shown to be improved when the samples were sintered at 950℃. The dominant mass transport mechanism appears to be grain-boundary diffusion during heat treatment at 950℃.

• 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.

• 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.16 no.8
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• pp.503-510
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• 2006

The measurement of specific gases is based on the reversible conductivity change of sensing materials in semiconductor type gas sensors. For an application as gas sensors of high sensitivity, porous $SnO_2$ films have been fabricated by anodizing of pure Sn foil in oxalic acid and characteristics of anodic tin oxide films have been investigated. Pore diameter and distribution were dependent on process conditions such as electrolyte concentration, applied voltage, anodizing temperature, and time. Characteristics of anodic films were explained with current density-time curves.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.328-328
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• 2007

$SnO_2$ has a high potential for electric and electronic applications. We have anodized pure tin metal and nano porous tin oxide film was obtained on pure Sn. Nano porous tin oxide were grown by anodization in nonaqueous-base electrolytes at different potentials between 5 V and 100 V. Pore size of ~100nm was observed by FE-SEM. Pore sizes as a function of applied voltage and anodizing time were characterized. We obtained nano porous tin oxide film having an uniform pore size at low temperature. High specific surface area of $SnO_2$ will be very useful for gas sensor, lithium battery, and dye sensitized solar cell.

• Journal of the Korean Society for Heat Treatment
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• v.31 no.3
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• pp.111-119
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• 2018

We report the post-annealing effect of Sn doped ZnO (ZnO:Sn) thin film grown on sapphire (001) substrate using radio-frequency powder sputtering method. During thermal annealing in a vacuum atmosphere, the ZnO:Sn thin film is transformed into a porous thin film. Based on X-ray diffraction, scanning electron microscopy, and energy dispersive X-ray analyses, a possible mechanism for the production of pores is presented. Sn atoms segregate to form clusters that act as catalysts to dissociate Zn-O bonds. The Zn and O atoms subsequently vaporize, leading to the formation of pores in the ZnO:Sn thin film. We also found that Sn clusters were oxidized to form SnO or $SnO_2$ phases.

• Korean Journal of Materials Research
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• v.25 no.1
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• pp.27-31
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• 2015

This paper proposes a novel way of fabricating aligned porous Sn by freeze-drying of camphene slurry with stannic oxide ($SnO_2$) coated Sn powders. The $SnO_2$ coated Sn powders were prepared by surface oxidation of the initial and ball-milled Sn powders, as well as heat treatment of tin chloride coated Cu powders. Camphene slurries with 10 vol% solid powders were prepared by mixing at $50^{\circ}C$ with a small amount of oligomeric polyester dispersant. Freezing the slurry was done in a Teflon cylinder attached to a copper bottom plate cooled at $-25^{\circ}C$. Improved dispersion stability of camphene slurry and the homogeneous frozen body was achieved using the oxidized Sn powder at $670^{\circ}C$ in air after ball milling. The porous Sn specimen, prepared by freeze-drying of the camphene slurry with oxidized Sn powder from the heat-treated Sn/tin chloride mixture and sintering at $1100^{\circ}C$ for 1 h in a hydrogen atmosphere, showed large pores of about $200{\mu}m$, which were aligned parallel to the camphene growth direction, and small pores in their internal walls. However, $100{\mu}m$ spherical particles were observed in the bottom part of the specimen due to the melting of the Sn powder during sintering of the green compact.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2015.11a
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• pp.250-250
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• 2015

사람의 후각으로 감지할 수 없는 독성, 폭발성 가스로 인한 사고 발생률이 높아지면서 고감도의 가스 센서 필요성이 증가 되고 있다. 본 연구에서는 안정적인 가스 감지를 위해 물리기상증착의 다양한 공정 조건을 변화시켜 다공성 나노구조의 $SnO_2$ 가스 검지 전극층을 제작하였다. SEM 분석을 통하여 $SnO_2$ 가스 검지층이 다공성 나노 구조를 지님을 확인하였고, TEM 분석을 통하여 $SnO_2$ 입자간의 안정적인 접합을 확인하였다. 또한 다공성 나노 구조의 $SnO_2$를 가스 검지층으로 사용하여 가스센서를 제작하였고, 가스 농도에 따른 감도 변화를 확인 할 수 있었다.