• Journal of Powder Materials
• /
• v.23 no.1
• /
• pp.49-53
• /
• 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
• /
• v.23 no.12
• /
• pp.722-726
• /
• 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 the Korean institute of surface engineering
• /
• v.51 no.1
• /
• pp.47-53
• /
• 2018

Sn-based lithium-ion batteries have low cost and high theoretical specific capacity. However, one of major problem is the capacity fading caused by volume expansion during lithiation/delithiation. In this study, 3-dimensional foam structure of Cu-Sn alloy is prepared by co-electrodeposition including large free space to accommodate the volume expansion of Sn. The Cu-Sn foam structure exhibits highly porous and numerous small grains. The result of EDX mapping and XPS spectrum analysis confirm that Cu-Sn foam consists of $SnO_2$ with a small quantity of CuO. The Cu-Sn foam structure electrode shows high reversible redox peaks in cyclic voltammograms. The galvanostatic cell cycling performances show that Cu-Sn foam electrode has high specific capacity of 687 mAh/g at a current rate of 50 mA/g. Through SEM observation after the charge/discharge processes, the morphology of Cu-Sn foam structure is mostly maintained despite large volume expansion during the repeated lithiation/delithiation reactions.

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

• Journal of the Korean Ceramic Society
• /
• v.46 no.4
• /
• pp.429-435
• /
• 2009

In this study, we investigated microstructure and the CO gas sensing properties of Ag-CuO-$SnO_2$ thin films prepared by co-evaporation and subsequently thermal oxidation at air atmosphere. The sensitivity of a Cu-Sn films, thermally oxidized at $600^{\circ}C$, is strongly affected by the amount of Cu. At Cu:7 wt%-Sn:93 wt%, the film exhibited a maximum sensitivity of ${\sim}2.3$ to CO gas of 1000 ppm at $300^{\circ}C$. In contrast, the sensitivity of a Sn-Ag film did not change significantly with the amount of Ag. An enhanced sensitivity of ${\sim}3.7$ was observed in the film with a composition of Ag:3 wt%-Cu:4 wt%-Sn:93 wt%, when thermally oxidized at $600^{\circ}C$. In addition, this thin film shows a response time of ${\sim}80$ sec and a recovery time of ${\sim}450$ sec to 1000 ppm CO gas. The results demonstrate that the CO sensitivity of the Ag-CuO-$SnO_2$ thin films may be closely associated with coexistence of $SnO_2$ and SnO phase, decrease in average particle size, and a porous microstructure. We also suggest that co-evaporation and followed by thermal oxidation is a very simple and effective method to prepare oxide gas sensor thin films.

• Current Photovoltaic Research
• /
• v.10 no.2
• /
• pp.39-48
• /
• 2022

A Se-containing Cu/SnSe₂/ZnSe precursor was employed to introduce S to the precursor to form Cu₂ZnSn(S,Se)₄ (CZTSSe) film. The morphology of CZTSSe films strongly varied with two different pre-annealing environments: S and N₂. The CZTSSe film with S pre-annealing showed a dense morphology with a smooth surface, while that with N₂ pre-annealing showed a porous film with a plate-shaped grains on the surface. CuS and Cu₂Sn(S,Se)₃ phases formed during the S pre-annealing stage, while SnSe and Cu₂SnSe₃ phases formed during the N₂ pre-annealing stage. The SnSe phase formed during N₂ pre-annealing generated SnS₂ phase that had plate shape and severely aggravated the morphology of CZTSSe film. The power conversion efficiency of the CZTSSe solar cell with S pre-annealing was low (1.9%) due to existence of Zn(S.Se) layer between CZTSSe and Mo substrate. The results indicated that S pre-annealing of the precursor was a promising method to achieve a good morphology for large area application.

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

• Current Photovoltaic Research
• /
• v.1 no.2
• /
• pp.109-114
• /
• 2013

$Cu_2ZnSnS_4$ (CZTS) nanoparticles were synthesized by a solvothermal method using copper (II) acetate, zinc acetate, tin chloride, and sulfur in diethylenetriamine solvent. Binary sulfide particles such as CuS, ZnS, SnS, and $SnS_2$ were obtained at $180^{\circ}C$; single-phase CZTS nanoparticles were obtained at $280^{\circ}C$. CZTS nanoparticles with spherical shape and grain size of 40 to 60 nm were obtained at $280^{\circ}C$. In the middle of 180 and $280^{\circ}C$, CZTS and ZnS phases were found. The time variation of reaction at $280^{\circ}C$ revealed that an amorphous state formed first instead of binary phases and then the amorphous phase was converted to crystalline CZTS state; it is different reaction path way from conventional solid-state reaction path of which binary phases react to form CZTS. CZTS films deposited and annealed from single-phase nanoparticles showed porous microstructure and poor adhesion. This indicates that a combination of CZTS and other flux phase is necessary to have a dense film for device fabrication.

• Korean Journal of Materials Research
• /
• v.25 no.12
• /
• pp.708-712
• /
• 2015

This study reports the effects of $H_2S$ gas concentration on the properties of $Cu_2ZnSnS_4(CZTS)$ thin films. Specifically, sulfurization process with low $H_2S$ concentrations of 0.05% and 0.1%, along with 5% $H_2S$ gas, was studied. CZTS films were directly synthesized on Mo/Si substrates by chemical bath deposition method using copper sulfate, zinc sulfate heptahydrate, tin chloride dihydrate, and sodium thiosulfate pentahydrate. Smooth CZTS films were grown on substrates at optimized chemical bath deposition condition. The CZTS films sulfurized at low $H_2S$ concentrations of 0.05 % and 0.1% showed very rough and porous film morphology, whereas the film sulfurized at 5% $H_2S$ yielded a very smooth and dense film morphology. The CZTS films were fully crystallized in kesterite crystal form when they were sulfurized at $500^{\circ}C$ for 1 h. The kesterite CZTS film showed a reasonably good room-temperature photoluminescence spectrum that peaked in a range of 1.4 eV to 1.5 eV, consistent with the optimal bandgap for CZTS solar cell applications.

• Journal of Mechanical Science and Technology
• /
• v.20 no.4
• /
• pp.513-521
• /
• 2006

The performances of porous bearings under different operating conditions were experimentally investigated in this study. Material groups studied are 90%Cu + 10%Sn bronze and 1%C + % balance Fe iron-based self-lubricating P/M bearings at constant (85%) density. In the experiments, the variation of the coefficient of friction and wear ratio of those two different group materials for different sliding speeds, loads, and temperatures were investigated. As a result, the variation of the friction coefficient-temperature for both constant load, and constant sliding speed, friction coefficient-average bearing pressure, PV-wear loss and temperature-wear loss curves were plotted and compared with each other for two materials, separately. The test results showed that Cu-based bearings have better friction and wear properties than Fe-based bearings.