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Synthesis of Porous Cu-Sn by Freeze Drying and Hydrogen Reduction Treatment of Metal Oxide Composite Powders (금속산화물 복합분말의 동결건조 및 수소분위기 환원처리에 의한 Cu-Sn 다공체 제조)

  • Kim, Min-Sung;Yoo, Ho-Suk;Oh, Sung-Tag;Hyun, Chang-Yong
    • 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.

BaTiO3 Particles of Core-Shell Structure for Aqueous Paste to Avoid VOC Emission during MLCC Manufacturing Process (MLCC 제조공정에서 VOC배출 억제를 위한 수계 Paste용 BaTiO3 코팅분말의 합성)

  • Kim, Jin-Su;Choi, Guang J.
    • Clean Technology
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    • v.8 no.4
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    • pp.173-180
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    • 2002
  • As a primary material for MLCC, $BaTiO_3$ particles coated with two additives in a core-shell structure were prepared in this study. This composite powder can not only reduce the VOC emission during MLCC manufacture but also increase the density and reliability of electronic products. The additives were $Y_2O_3$ and $MnCO_3$, whose composition information was obtained from domestic companies. It was observed that the surface of $BaTiO_3$ particles was uniformly as well as simultaneously coated by those two materials via urea-decomposition reaction over $70^{\circ}C$ as the reaction temperature. Elemental analysis indicated that the measured content of each additve was quite close to the designated value. The effect of polymeric dispersant such as PVP, on the coating characteristics was not as significant as expected.

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Functional Ingredients of Perilla Frutescens L. Britt Extracts and Preparation of PVA Nanoweb Containing Extracts (자소 추출물의 기능성 성분과 자소 추출물을 함유하는 PVA 나노 섬유의 제조)

  • Wang, Qian Wen;Lee, Jung-Soon
    • Textile Coloration and Finishing
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    • v.29 no.4
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    • pp.256-267
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    • 2017
  • The purpose of this study was to analyze the functional ingredients of Perilla Frutescens L. Britt extracts and to confirm the possibility of producing PVA nanofibers using extracts. Distilled water, 3% aqueous sodium hydroxide solution and ethanol were used as extraction solvents. The electrospinning was carried out at a PVA concentration of 12%, an applied voltage of 10 kV and a tip to collector distance of 15cm. The contents of volatile substances, essential oils, total polyphenols and flavonoids of the extracts were measured to examine the constituents of functional materials. Flavor components and esters were identified in 3% sodium hydroxide and ethanol extracts. The content of polyphenols and flavonoids in ethanol extracts was higher than that of medicinal plants. 1wt.% of Tween 20 was added to disperse the essential oil components of the ethanol extract. Addition of a dispersant made it possible to produce a homogeneous mixture by having some compatibility with the ethanol extracts and the PVA molecule. When the concentration of the ethanol extract was 0.25 and 0.5wt%, relatively uniform PVA nanofiber having an average diameter of 350 to 365nm could be produced. The results of FT-IR, XRD and DSC analysis confirmed that Perilla Frutescens L. Britt ethanol extract was well mixed with PVA molecules and was electrospun.

Preparation and Characterization of Silicone and Fluorine-Oil-Based Ferrofluids

  • Kim, Jong-Hee;Park, Keun-Bae;Kim, Ki-Soo
    • Composites Research
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    • v.30 no.1
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    • pp.41-45
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    • 2017
  • Magnetite nanoparticles were synthesized by adding an ammonium hydroxide to a mixed solution of iron (II) and (III) chlorides. A silicon surfactant of ${\alpha},{\omega}$-(3-aminopropyl)polydimethylsiloxane was adsorbed on the particles as dispersant and a polydimethylsiloxane polymer was used to prepare ferrofluids of silicone oil base. Fluorinated surfactants of anionic ammoniated perfluoroalkyl sulfonamide and nonionic fluoroaliphatic polymeric esters were applied to the particles and a perfluoropolyether was used to prepare ferrofluids of fluorine oil base. The experimental conditions were used for preparing the ferrofluids with concentrations of 200, 300 and 400 mg/mL, and density, magnetization and viscosity of the products were characterized. The density values increased in proportion to the concentration, indicating 1.11-1.27 g/mL for silicone-oil-based fluids and 1.95-2.10 g/mL for fluorine-oil-based fluids in the range of 200-400 mg/mL. The saturation magnetization of the silicone-oil-based and fluorine-oil-based fluids indicated 14.7, 24.4, and 30.7 mT and 15.8, 23.3, and 33.7 mT for 200, 300, and 400 mg/mL, respectively, depending on the content of magnetic particles in the fluid. The viscosity of the silicone-oil-based ferrofluids was highly stable compared to that of the fluorine-oil-based with increasing temperatures. The ferrofluids are usually applied to seals and speakers with the silicone base and to seals with the fluorine base.

Fabrication and Properties of Porous Tungsten by Freeze-Drying Process (동결건조 공정을 이용한 텅스텐 다공체의 제조 및 특성)

  • Lee, Young-Sook;Oh, Sung-Tag
    • Korean Journal of Materials Research
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    • v.21 no.9
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    • pp.520-524
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    • 2011
  • Porous W with controlled pore characteristics was fabricated by a freeze-drying process. $WO_3$ powder and camphene were used as the source materials of W and sublimable vehicles, respectively. Camphene slurries with $WO_3$ contents of 10 and 15 vol% were prepared by milling at $50^{\circ}C$ with a small amount of oligomeric polyester dispersant. Freezing of a slurry was done in a Teflon cylinder attached to a copper bottom plate cooled 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 body was hydrogen-reduced at $800^{\circ}C$ for 30 min and sintered in a furnace at $900^{\circ}C$ for 1 h under a hydrogen atmosphere. Microstructural observation revealed that all of the sintered samples were composed of only W phase and showed large pores which were aligned parallel to the camphene growth direction. The porosity and pore size increased with increasing camphene content. The difference in the pore characteristics depending on the slurry concentration may be explained by the degree of powder rearrangement in the slurry. The results strongly suggest that a porous metal with the required pore characteristics can be successfully fabricated by a freeze-drying process using metal oxide powders.

Fabrication of Porous Ti by Freeze-Drying and Heat Treatment of TiH2/Camphene Slurries (TiH2/camphene 슬러리의 동결건조 및 열처리에 의한 Ti 계 다공체의 제조)

  • Seo, Han Gil;Kim, Young Do;Suk, Myung-Jin;Oh, Sung-Tag
    • Korean Journal of Materials Research
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    • v.23 no.6
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    • pp.339-343
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    • 2013
  • Porous Ti-systems with unidirectionally aligned channels were synthesized by freeze-drying and a heat treatment process. $TiH_2$ powder and camphene were used as the source materials of Ti and sublimable vehicles, respectively. Camphene slurries with $TiH_2$ content of 10 and 15 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 at $-25^{\circ}C$ while unidirectionally controlling the growth direction of the camphene. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green body was heat-treated at $1100^{\circ}C$ for 1 h in a nitrogen and air atmosphere. XRD analysis revealed that the samples composed of TiN and $TiO_2$ phase were dependent on the heat-treatment atmosphere. The sintered samples showed large pores of about 120 mm which were aligned parallel to the camphene growth direction. The internal wall of the large pores had relatively small pores with a dendritic structure due to the growth of camphene dendrite depending on the degree of nucleation and powder rearrangement in the slurry. These results suggest that a porous body with an appropriate microstructure can be successfully fabricated by freeze-drying and a controlled sintering process of a camphene/$TiH_2$ slurry.

Particle Behavior and Properties of Pigment Red 57:1 Synthesized in Various Reaction Conditions (다양한 반응 조건에 따른 적색안료 57:1의 입자거동 및 특성)

  • Yang, Seok Won;Kim, Jae Hwan;Kim, Do Hyun;Jin, Young Eup;Lee, Gun-Dae;Park, Seong Soo
    • Applied Chemistry for Engineering
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    • v.28 no.1
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    • pp.95-100
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    • 2017
  • In this study, various Pigment Red 57:1 samples and also their dispersant were prepared in various synthesis conditions via changing parameters such as synthesis time, pH, derivative content and synthesis temperature in order to analyze the pigment particle behaviors and their spectroscopic and physical properties. Each sample was analyzed using Fourier infrared spectroscopy, UV-Vis spectroscopy, particle size analyzer, color spectrophotometer and X-ray diffractometer and their characteristics were compared. As a result, it was possible to control the size of pigment particles by controlling the synthesis conditions.

Synthesis and Microstructure of Porous Al2O3 with Nano-Sized Cu Dispersions (나노크기 Cu 분산입자를 갖는 Al2O3 다공체의 제조 및 미세조직 특성)

  • Yoo, Ho-Suk;Kim, An-Gi;Hyun, Chang-Yong
    • 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.

Printing Properties of Ag Paste with the Variation of Binder on the SiNx Coated Si Wafer (SiNx 층이 코팅된 Si Wafer에 바인더 종류에 따른 Ag 페이스트의 인쇄 특성)

  • Kang, Jea Won;Shin, Hyo Soon;Yeo, Dong Hun;Jeong, Dae Yong
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.27 no.2
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    • pp.85-90
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    • 2014
  • Ag paste has been used in the front electrode of the Si-solar cell. It is composed by Ag powder, glass frit, binder, solvent and dispersant. The role of the binder and the solvent is to make a flow and a printing property. However, it was not enough to report the printing properties with the variation of binder in the controled viscosity. In this study, we selected 3 kinds of typical binder which were used as binder for the paste in the industry, such as Ethyl cellulose, Hydroxypropyl cellulose and Acrylic. Ag pastes using these were prepared, controled viscosity and printed on the SiNx coated Si wafer. In the 'A paste' used Acrylic binder, printed hight was highest and 'H paste' used Hydroxypropyl cellulose binder was lowest. Because 'H paste' was high viscosity due to the molecular weight, the solvent was added in the paste to control the viscosity. Therefore, the content of solid was lower in 'H paste'. The relative pattern width which is related to the spreading of paste was the best in the case of 'H paste' and 'EH paste' at $30^{\circ}C$. It is thought that the optimization of the relative pattern width is possible for a paste by the controling shear thinning phenomenon. In the case of 'A paste', though printing hight was best, the pattern width was dependant on the temperature.

Effect of Tert-Butyl Alcohol Template on the Pore Structure of Porous Tungsten in Freeze Drying Process (동결건조 공정에서 Tert-butyl alcohol 기공형성제가 텅스텐 다공체의 기공구조에 미치는 영향)

  • Lee, Eui Seon;Heo, Youn Ji;Ko, Yun Taek;Park, Jin Gyeong;Cho, Yong-Ho;Oh, Sung-Tag
    • 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.