• Title/Summary/Keyword: Liquid phase reduction process

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Synthesis of Nano Sized Cobalt Powder from Cobalt Sulfate Heptahydrate by Liquid Phase Reduction (액상환원공정을 이용한 황산코발트로부터의 코발트 나노분말 합성)

  • An, Se-Hwan;Kim, Se-Hoon;Lee, Jin-Ho;Hong, Hyun-Seon;Kim, Young-Do
    • Korean Journal of Materials Research
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    • v.21 no.6
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    • pp.327-333
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    • 2011
  • Nanostructured cobalt materials have recently attracted considerable attention due to their potential applications in high-density data storage, magnetic separation and heterogeneous catalysts. The size as well as the morphology at the nano scale strongly influences the physical and chemical properties of cobalt nano materials. In this study, cobalt nano particles synthesized by a a polyol process, which is a liquid-phase reduction method, were investigated. Cobalt hydroxide ($Co(OH)_2$), as an intermediate reaction product, was synthesized by the reaction between cobalt sulphate heptahydrate ($CoSO_4{\cdot}7H_2O$) used as a precursor and sodium hydroxide (NaOH) dissolved in DI water. As-synthesized $Co(OH)_2$ was washed and filtered several times with DI water, because intermediate reaction products had not only $Co(OH)_2$ but also sodium sulphate ($Na_2SO_4$), as an impurity. Then the cobalt powder was synthesized by diethylene glycol (DEG), as a reduction agent, with various temperatures and times. Polyvinylpyrrolidone (PVP), as a capping agent, was also added to control agglomeration and dispersion of the cobalt nano particles. The optimized synthesis condition was achieved at $220^{\circ}C$ for 4 hours with 0.6 of the PVP/$Co(OH)_2$ molar ratio. Consequently, it was confirmed that the synthesized nano sized cobalt particles had a face centered cubic (fcc) structure and with a size range of 100-200 nm.

Shape Control of Platinum Nanoparticles Using a Metal Salt (금속 염을 이용한 백금 나노입자의 형상제어)

  • Kwak, Seoung Yeul;Lee, Jin Ho;Kim, Jin Woo;Jung, Taek Kyun;Kim, Young Do
    • Journal of Powder Materials
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    • v.19 no.6
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    • pp.393-397
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    • 2012
  • $AgNO_3$ has the characteristic is controlling the inhibition or promotion of particle growth by adsorbing onto specific facets of platinum nanoparticles. Therefore, in this study, $AgNO_3$ was added to control the shape of platinum nanoparticles during the liquid phase reduction process. Consequently, platinum cubes were synthesized when $AgNO_3$ of 1.1 mol% (with respect to the Pt concentration) was added into the solution. Platinum octahedrons were synthesized when 32 mol% (with respect to the Pt concentration) was added into the solution. These results demonstrate that the metal salt $AgNO_3$, effectively controlled the relative growth rates of each facet of Pt nano particles.

Densification of Cu-50%Cr Powder Compacts and Properties of the Sintered Compacts (Cu-50%Cr 분말성형체의 치밀화 및 소결체 물성)

  • 김미진;정재필;도정만;박종구;홍경태
    • Journal of Powder Materials
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    • v.7 no.4
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    • pp.218-227
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    • 2000
  • It is well known that the Cu-Cr alloys are very difficult to be made by conventional sintering methods. This difficulty originates both from limited solubility of Cr in the Cu matrix and from limited sintering temperature due to high vapor pressures of Cr and Cu components at the high temperature. Densification of Cu-50%Cr Powder compacts by conventional Powder metallurgy Process has been studied. Three kinds of sintering methods were tested in order to obtain high-density sintered compacts. Completely densified Cu-Cr compacts could be obtained neither by solid state sintering method nor by liquid phase sintering method. Both low degree of shrinkage and evolution of large pores in the Cu matrix during the solid state sintering are attributed to the anchoring effect of large Cr particles, which inhibits homogeneous densification of Cu matrix and induces pore generation in the Cu matrix. In addition, the effect of undiffusible gas coming from the reduction of Cu-oxide and Cr-oxide was observed during liquid phase sintering. A two-step sintering method, solid state sintering followed by liquid phase sintering, was proved to have beneficial effect on the fabrication of high-dendsity Cu-Cr sintered compacts. The sintered compacts have properties similar to those of commercial products.

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Fabrication of Metallic Particle Dispersed Ceramic Based Nanocomposite Powders by the Spray Pyrolysis Process Using Ultrasonic Atomizer and Reduction Process

  • Choa, Y.H.;Kim, B.H.;Jeong, Y.K.;Chae, K.W.;T.Nakayama;T. Kusunose;T.Sekino;K. Niibara
    • Journal of Powder Materials
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    • v.8 no.3
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    • pp.151-156
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    • 2001
  • MgO based nanocomposite powder including ferromagnetic iron particle dispersions, which can be available for the magnetic and catalytic applications, was fabricated by the spray pyrolysis process using ultra-sonic atomizer and reduction processes. Liquid source was prepared from iron (Fe)-nitrate, as a source of Fe nano-dispersion, and magnesium (Mg)-nitrate, as a source of MgO materials, with pure water solvent. After the chamber were heated to given temperatures (500~$^800{\circ}C$), the mist of liquid droplets generated by ultrasonic atomizer carried into the chamber by a carrier gas of air, and the ist was decomposed into Fe-oxide and MgO nano-powder. The obtained powders were reduced by hydrogen atmosphere at 600~$^800{\circ}C$. The reduction behavior was investigated by thermal gravity and hygrometry. After reduction, the aggregated sub-micron Fe/MgO powders were obtained, and each aggregated powder composed of nano-sized Fe/MgO materials. By the difference of the chamber temperature, the particle size of Fe and MgO was changed in a few 10 nm levels. Also, the nano-porous Fe-MgO sub-micron powders were obtained. Through this preparation process and the evaluation of phase and microstructure, it was concluded that the Fe/MgO nanocomposite powders with high surface area and the higher coercive force were successfully fabricated.

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Fabrication and Characterization of Ag Particles by Polyol Process and Wet Chemical Process (폴리올 공정과 액상 환원 공정에 따른 은 입자 제조 및 특성 평가)

  • Yoo, Juyeon;Jang, Hyosung;Lee, Kun-Jae
    • Journal of Powder Materials
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    • v.23 no.4
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    • pp.297-302
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    • 2016
  • Ag nanoparticles are extensively studied and utilized due to their excellent catalysis, antibiosis and optical properties. They can be easily synthesized by chemical reduction methods and it is possible to prepare particles of uniform size and high purity. These methods are divided into vapor methods and liquid phase reduction methods. In the present study, Ag particles are prepared and analyzed through two chemical reduction methods using solvents containing a silver nitrate precursor. When Ag ions are reduced using a reductant in the aqueous solution, it is possible to control the Ag particle size by controlling the formic acid ratio. In addition, in the Polyol process, Ag nanoparticles prepared at various temperatures and reaction time conditions have multiple twinned and anisotropic structures, and the particle size variation can be confirmed using field emissions scanning electron microscopy and by analyzing the UV-vis spectrum.

A study on the synthesis of tin oxide crystalline by the liquid reduction precipitation method and hydrothermal process (액상환원침전법 및 수열반응법을 이용한 주석산화물 결정 합성에 관한 연구)

  • Park, Il-Jeong;Kim, Geon-Hong;Kim, Dae-Weon;Choi, Hee-Lack;Jung, Hang-Chul
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.3
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    • pp.95-100
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    • 2016
  • In this work, tin oxides were obtained by the liquid reduction precipitation method and hydrothermal process using $SnCl_2{\cdot}2H_2O$, $N_2H_4$, and NaOH. Tin oxide crystals having different sizes and morphologies could be achieved. The powders were characterized by X-ray diffraction (XRD) and Field Emission Scanning Electron Microscopy (FE-SEM). Depending on the molar ratio of the raw materials, tin oxide crystalline with the spherical and rectangular plate-like shape could be obtained, the crystal phase was SnO and $Sn_6O_4(OH)_4$. And the obtained SnO crystals by a hydrothermal reaction showed various shapes, such as, spherical, plate-like and flower-like architectures depending on the temperature conditions.

Finite Element Analysis of Extrusion Process in Semi-Solid State (반용융 재료의 압출공정에 관한 유한요소 해석)

  • Hwang, Jae-Ho;Go, Dae-Cheol;Min, Gyu-Sik;Kim, Byeong-Min;Choe, Jae-Chan
    • Transactions of Materials Processing
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    • v.7 no.4
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    • pp.364-374
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    • 1998
  • It is the objective of this study to analyze the effect of various process variables on the quality of extruded product and extrusion force for semi-solid extrusion of Al2024 with solid phase structure of globular type by the finite element method. Process variables are initial solid fraction, ram speed, semi-angle of die, and reduction in area. The results of experiment are compared with those of simulation in order to verify the usefulness of the developed finite element program. The flow and deformation of semi-solid alloy are analyzed by coupling by coupling the deformation of porous skeleton and the flow of liquid phase. It is also assumed that initial solid fraction is homogeneous.

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A Study on the Sludge Reduction and Biogas Production through a Two-phase Anaerobic Digestion Process (이상 혐기성 소화 공정을 통한 슬러지 발생량 저감과 바이오가스 생산에 관한 연구)

  • Woo, Mi-Hee;Han, Gee-Bong
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.9
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    • pp.894-899
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    • 2010
  • We coordinated the experiments with ozone pretreatment and two-phase anaerobic digestion using solid-liquid separation to raise the efficiency of sludge volume reduction and obtained the following results. The pre-treatment with ozone reduced the solid concentration in the average of TSS $8.3{\pm}2.0%$ TSS and $9.2{\pm}}2.8%$ VSS. Of the organic material, TCOD decreased $5.1{\pm}2.4%$, but SCOD showed $72{\pm}6.5%$ increased, which was due to destruction of the cell wall and dissolution of icell media by the powerful oxidative stress of ozone. During the two-phase anaerobic digestion process, we achieved the reduction of $21.5{\pm}3.4%$ TSS, $20.2{\pm}8.4%$ VSS, $32.1{\pm}7.9%$ TCOD and $22.1{\pm}7.2%$ SCOD in average. The maximum methane gas production were 177.6 mL per g TSS, 210.8 mL per g VSS, 127.0 mL per g TCOD and 1452.0 mL per g SCOD, respectively. Solid material reduction through the two-phase anaerobic digestion and MLE (Modified Ludzack-Ettinger) processes were 93.8% of TSS and 92.0% of VSS. We concluded that suggested two-phase anaerobic digestion and MLE process could achieve the reasonable production of biogas and a maximum reduction of the sludge volume.

Synthesis of NiTi Alloy Powder by the Reaction of NiO-TiH2 Mixing Powders (NiO-TiH2 혼합분말의 반응을 이용한 NiTi 합금분말 제조)

  • Jeon, Ki Cheol;Lee, Han-Eol;Yim, Da-Mi;Oh, Sung-Tag
    • Journal of Powder Materials
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    • v.22 no.4
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    • pp.266-270
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    • 2015
  • The synthesis of NiTi alloy powders by hydrogen reduction and dehydrogenation process of NiO and $TiH_2$ powder mixtures is investigated. Mixtures of NiO and $TiH_2$ powders are prepared by simple mixing for 1 h or ball milling for 24 h. Simple-mixed mixture shows that fine NiO particles are homogeneously coated on the surface of $TiH_2$ powders, whereas ball milled one exhibits the morphology with mixing of fine NiO and $TiH_2$ particles. Thermogravimetric analysis in hydrogen atmosphere reveals that the NiO and $TiH_2$ phase are changed to metallic Ni and Ti in the temperature range of 260 to $290^{\circ}C$ and 553 to $639^{\circ}C$, respectively. In the simple-mixed powders by heat-up to $700^{\circ}C$, agglomerates with solid particles and solidified liquid phase are observed, and the size of agglomerates is increased at $1000^{\circ}C$. From the XRD analysis, the presence of liquid phase is explained by the formation and melting of $NiTi_2$ inter-metallic compound due to an exothermic reaction between Ni and Ti. The simple-mixed powders, heated to $1000^{\circ}C$, lead to the formation of NiTi phase but additional Ni-, Ti-rich and Ti-oxide phases. In contrast, the microstructure of ball-milled powders is characterized by the neck-grown particles, forming $Ni_3Ti$, Ti-oxide and unreacted Ni phase.

Study on the Behavior Characteristics of the Evaporative Diesel Spray under Change in Ambient Conditions (주위조건 변화에 대한 증발 디젤분무 거동특성 연구)

  • Yeom, Jeong-Kuk
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.33 no.6
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    • pp.454-460
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    • 2009
  • To analyze the mixture formation process of evaporating diesel spray is important for emissions reduction in actual engines. Then the effects of change in density of ambient gas on spray structure in high temperature and pressure field have been investigated in this study. The ambient gas density was changed from ${\rho}_a=5.0kg/m^3$ to ${\rho}_a=12.3kg/m^3$ with CVC(Constant Volume Chamber). Also, simulation study by modified KIVA-II code was conducted and compared with experimental results. The ambient temperature and injection pressure are kept as 700K and 72MPa, respectively. The images of liquid and vapor phase in the evaporating free spray were simultaneously taken by exciplex fluorescence method. As experimental results, with increasing ambient gas density, the tip penetration of the evaporating free spray decreases due to the increase in the drag force from ambient gas. The spatial structure of a diesel spray can be verified as 2-regions consisted of liquid with momentum decrease and vapor with large-scale vortex. The calculated results obtained by modified KIVA-II code show good agreements with experimental results.