• Title/Summary/Keyword: 습식화학합성

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Fabrication of Cu Flakes by Ball Milling of Sub-micrometer Spherical Cu Particles (서브 마이크론급 구형 동분말의 볼 밀링을 통한 플레이크 동분말의 제조)

  • Kim, Ji Hwan;Lee, Jong-Hyun
    • Journal of the Microelectronics and Packaging Society
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    • v.21 no.4
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    • pp.133-137
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    • 2014
  • As a preceding process for preparing several micrometer sized Ag-coated Cu flakes, ball milling of submicrometer-sized Cu particles synthesized through a wet chemical method was performed in order to convert the particles into flakes. To suppress oxidation and aggregation of the particles during ball milling, ethylene glycol and ethyl acetate were used as a medium and a surface modifying agent, respectively. Results obtained with different rotation speeds of a jar indicated that the rotation speed changes a rotating mode, and strikingly alters the final shapes and shape uniformity of Cu particles after milling. The diameter of zirconia ball was also confirmed. Although there was aggregates in the initial submicrometer-sized Cu particles, therefore, well-dispersed Cu flakes with a size of several micrometers were successfully prepared by ball milling through optimization of rotation speed, amount of ethyl acetate, and diameter of zirconia ball.

Surface Treatment of IHX Materials for VHTR (원자력 중간열교환기 열수송계 소재의 표면처리)

  • Lee, Byeong-U;Lee, Myeong-Hun;Bang, Gwang-Hyeon
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2012.11a
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    • pp.35-50
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    • 2012
  • $900^{\circ}C$이상 초고온 He-gas 분위기 또는 용융불화염 (molten salts, FLINAK) 환경에서 사용될 VHTR(Very High Temperature Reactor)의 IHX(Intermediate heat exchanger)용 열수송 구조재료로 가장 가능성이 높은 합금인 Inconel 617 및 Hastelloy X 상에 습식화학적, 물리적기상합성법(Vacuum arc-plasma과 RF magnetron sputtering) 및 pack cementation에 의한 표면개질 및 마이크로 초내열(refractory ceramics) 코팅층(TiN, TiCN, TiAlN, $Al_2O_3$, $TiO_2$)을 형성시켰다. 고온 장기사용 시 문제가 될 수 있는 고온에서의 조직변화, 미세구조와 상(phase)형성, 고온 부식 및 그에 따른 마모(wear resistance) 손상 등 이들 소재의 내열, 내식 및 내마모 물성을 개선하는 연구를 수행하였다. TiAlN 박막의 경우 공기분위기에서 N이 분해되나 치밀한 산화물($TiO_2/Al_2O_3$ layer)을 형성하여 내식성 있는 보호피막을 형성함으로 기판과의 열팽창 계수로 인한 박리가 발생하지 않아 보호피막으로 적합하였다. Pack cementation법에 의한 aluminiding(Al-Ni합금)도 He 및 공기분위기에서 고온물성의 저하를 가져오는 $Cr_2O_3$의 생성을 충분히 억제하고 있었으며 He 및 air 분위기에서 사용이 가능한 박막으로 여겨진다. 내열 및 내식성에 대한 실험을 종합한 결과, 공기분위기에서 사용할 수 없는 박막은 He-gas 및 FLINAK(LiF-NaF-KF) 용융염 분위기에서도 사용할 수 없었으며, He-gas, FLINAK 및 air 분위기에서 모두 사용이 가능한 박막으로는 Inconel 617에서는 $(TiO_2-)Al_2O_3$, TiAlN 및 Al-Ni이었고 Hastelloy에서는 Al-Ni 및 $Al_2O_3$가 가장 적당하였다.

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Characteristics of methane reforming with carbon dioxide using transition metal catalyts (전이금속 촉매를 이용한 이산화탄소와 메탄의 개질 특성)

  • Jang, Hyun Tae
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.22 no.2
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    • pp.644-650
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    • 2021
  • This study characterized the reforming of methane with carbon dioxide, which is a major cause of global warming. The methane decomposition reaction with carbon dioxide was carried out using transition metal catalysts. The reactivity of tin was lower than that of a transition metal, such as nickel and iron. Most of the decomposition reaction occurred in the solid state. The melting point of tin is 505.03 K. Tin reacts in a liquid phase at the reaction temperature and has the advantage of separating carbon produced by the decomposition of methane from the liquid tin catalyst. Therefore, deactivation due to the deposition of carbon in the liquid tin can be prevented. Methane decomposition with carbon dioxide produced carbon monoxide and hydrogen. Ni was used to promote the catalyst performance and enhance the activity of the catalyst and lifetime. In this study, catalysts were synthesized using the excess wet impregnation method. The effect of the reaction temperature, space velocity was measured to calculate the activity of catalysts, such as the activation energy and regeneration of catalysts. The carbon-deposited tin catalyst regeneration temperature was 1023 K. The reactivity was improved using a nickel co-catalyst and a water supply.

Measurements of the Temperature Coefficient of Resistance of CVD-Grown Graphene Coated with PEI (PEI가 코팅된 CVD 그래핀의 저항 온도 계수 측정)

  • Soomook Lim;Ji Won Suk
    • Composites Research
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    • v.36 no.5
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    • pp.342-348
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    • 2023
  • There has been increasing demand for real-time monitoring of body and ambient temperatures using wearable devices. Graphene-based thermistors have been developed for high-performance flexible temperature sensors. In this study, the temperature coefficient of resistance (TCR) of monolayer graphene was controlled by coating polyethylenimine (PEI) on graphene surfaces to enhance its temperature-sensing performances. Monolayer graphene grown by chemical vapor deposition (CVD) was wet-transferred onto a target substrate. To facilitate the interfacial doping by PEI, the hydrophobic graphene surface was altered to be hydrophilic by oxygen plasma treatments while minimizing defect generation. The effect of PEI doping on graphene was confirmed using a back-gated field-effect transistor (FET). The CVD-grown monolayer graphene coated with PEI exhibited an improved TCR of -0.49(±0.03) %/K in a temperature range of 30~50℃.

Preparation and properties of water-based magnetic fluid with synthesized magnetite (합성마그네타이트를 이용한 수상자성유체의 제조 및 특성)

  • Kim, Mahn;Oh, Jae-Hyun;Seo, Ho-Jun;Cho, Moung-Ho;Kim, Mi-Sung
    • Journal of the Korean Magnetics Society
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    • v.4 no.2
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    • pp.173-178
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    • 1994
  • The water-based magnetic fluids were prepared with the synthesized ultra-fine magnetite, oleic acid and SDBS (sodium dodecyl benzene sulfonate) as surfactants. The dispersion of water-based magnetic fluids was about 90 % when the added amounts of oleic acid and SDBS for magnetite(27 g) were more than $2.66{\times}10^{-3}$ mol and 10 g respectively. As the solid content increased from o. 05 g/cc to 0.4 g/cc, saturation magnetization of magnetic fluids at 5 kOe increased from 1.98 emu/g to 9.63 emu/g at $Fe^{2+}/Fe^{3+}=0.5$ and from 2.7 emu/g to 14.63 emu/g at $Fe^{2+}/Fe^{3+}=1.0$, and the its viscosity increased from 1.3 cp to 4.4 cp at $Fe^{2+}/Fe^{3+}=0.5$. pH region of oleic acid and SDBS stabilized water-based mag¬netic fluids was stable was in the range of pH 3.0 to pH 11.0. Stability of Water-based magnetic fluids can be obtained by observation of magnetic memory patterns on the VCR tape.

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Investigation of Spherical LiMn2O4 Cathode Materials by Spray-drying with Different Electrochemical Behaviors at High Rate (분무건조법으로 제조한 구형 스피넬계 LiMn2O4 양극소재의 합성 조건에 따른 고출력 거동에 대한 연구)

  • Song, Jun Ho;Cho, Woosuk;Kim, Young Jun
    • Journal of the Korean Electrochemical Society
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    • v.19 no.2
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    • pp.50-56
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    • 2016
  • Spherical lithium manganese oxide spinel, $Li_{1.10}Mn_{1.86}Al_{0.02}Mg_{0.02}O_4$ was prepared by wet-milling, spray-drying, and sintering process. In the spray-drying process, solid content in slurry was varied from 20 to 30 wt%. In the sintering process, the precursors have been sintered under air or $O_2$ atmosphere. While the as-prepared samples exhibit excellent electrochemical properties at room temperature, the discharge voltage profiles at 5.0C are very different one from another. The origin for the difference especially at initial state of discharge is oxygen defect. The sample prepared in air has larger capacity related to the plateau at 3.3 V (vs. $Li/Li^+$) which is caused by the oxygen defects than the one prepared in $O_2$. The difference of discharge voltage profiles especially at the final state of discharge comes from different diffusion rate of $Li^+$ ions. The sample prepared from 30 wt% solid content of slurry shows twice higher diffusion rate than the samples prepared from 20 wt% solid content, which is attributed to better compactness between primary particles for the sample prepared from 30wt % solid content than the one prepared by 20 wt%.

Relationship between Particle Density and Electrochemical Properties of Spherical LiMn2-xMxO4 (M = Al, Mg, B) Spinel Cathode Materials (구형 스피넬계 LiMxMn2-xO4 (M = Al, Mg, B) 양극소재의 입자치밀도와 전지성능간의 상관관계에 대한 연구)

  • Kim, Kyoung-Hee;Jung, Tae-Gyu;Song, Jun-Ho;Kim, Young-Jun
    • Journal of the Korean Electrochemical Society
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    • v.15 no.2
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    • pp.67-73
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    • 2012
  • Spherical lithium manganese oxide spinel, $LiMn_{2-x}M_xO_4$ (M = Al, Mg, B) prepared by wet-milling, spray-drying, and sintering process has been investigated as a cathode material for lithium ion batteries. As-prepared powders exhibit various surface morphologies and internal density in terms of boron (B) doping level. It is found that the dopant B drives the growth of the primary particle and minimizes the surface area of the powder. As a result, the dopant enhances the internal density of the particles. Electrochemical tests demonstrated that the capacity of the synthesized material at 5 C could be maintained up to 90% of that at 0.2 C. The cycle performance of the material showed that the initial capacity was retained up to 80% even after 500 cycles under the high temperature of $60^{\circ}C$.

Fabrication of high purified zirconium dioxide (ZrO2) and stabilized zirconia (TZP: tetragonal zirconia polycrystal) powders (고순도 산화지르코늄(ZrO2) 및 안정화 지르코니아 (TZP: tetragonal zirconia polycrystal) 분말제조)

  • 최의석
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06b
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    • pp.55-85
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    • 1996
  • 지르코니아 분말은 ZrO2 결정상이 온도변화에 따라 부피변화를 수반하는 상전이변태를 나타낸다. 단사정 ZrO2가 110$0^{\circ}C$에서는 정방정으로, 2$700^{\circ}C$ 내외에서는 입방정으로 결정구조가 가역적으로 변한다. 이 ZrO2에 금속산화물을 고용시키면 형석 (CaF2:Florite)형의 입방정 결정구조가 실온에서도 안정하게 존재하게 된다. 안정화제 산화물은 caO, MgO등 2가 산화물외에 3가 또는 4가의 금속산화물로서 Sc2O3, Y2O3, Sm2O3, Nd2O3, Gd2O3, Y2O3, CeO2 등이며 이들은 금속이온의 원자가가 변하기 쉬운 희토류 산화물이다. 안정화 지르코니아는 형석형 결정구조이며 결정화학적으로 보면 금속양이온이 산소이온에 대해서 정육면체형의 8배위를 하고 있다. 이때 이온반경비(양이온/음이온)에 따라 Zr+4자리와 O-2자리의 격자위치와 모양이 형성되므로 비틀어진 정육면체구조이건 이상적인 정육면체 형석구조를 이룬다. 이는 지르코니아의 결정상의 2상-3상인 부분안정화 지르코니아다결정체(PSZ : partially stabilized zirconia)이거나 단일상-2상인 정방정 지르코니아다결정체(TZP : tetragonal zirconia polycrystal)의 결정구조를 가지는데 기인한다. PSZ는 주로 MgO, CaO를 안정화제로 고용시켜 입방정 영역에서 소결하고 이를 다시 입방정과 정방정의 상 영역에서 열처리하여 입방정 입자내부에 정방정을 석출 형성시킨 것이며 TZP는 Y2O3 및 CeO2를 고용시켜 PSZ와 다르게 일반적인 상압소결한 정방정 결정상의 미립자이다. 산화지르코늄 분말은 지르콘사에서 열분해시킨 지르코늄소결.융해괴(caustic fusion clinker)를 산처리하여얻어진 지르코늄산용액(zirconyl acid solution : cloride, sulfide, nitride 등)으로부터 제조된다. 고순도 산화지르코늄은 용액 결정석출법에 의해 ZrOCl2.8H2O, 5ZrO2.3SO3.15H2O, ZrO(NO3)2.xH2O 등의 지르코늄 수화물만을 재결정화시킨 것으로부터 얻을 수 있으며 이 지르코늄염 수용액으로부터 입자미세구조를 효과적으로 제어하여 산화지르코늄 및 안정화 지르코니아 분말제조가 가능하다. 안정화 지르코니아 분말은 ZrO2와 안정화산화물의 고용을위하여 가열처리를 필요로 하며 일정온도에서 최적상태로 숙성하므로서 2가지 상(phase) 이상의 고용체를 가지게 된다. 안정화 지르코니아 분말은 고용처리온도를 낮추고 효과적으로 생성시키기 위해서는 지르코늄 및 안정화제염을 혼합하고 습식 직접합성하여 저온에서 고용체의 합해진상 영역을 생성시키는 것이다. 이는 지르코니아 원료분말의 미세구조를 제어하므로서 가능하며 이때 화학성분조성과 크기형태가 균일하게 분포된 입자분말을 얻을 수 있다.

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Numerical and Experimental Study on the Coal Reaction in an Entrained Flow Gasifier (습식분류층 석탄가스화기 수치해석 및 실험적 연구)

  • Kim, Hey-Suk;Choi, Seung-Hee;Hwang, Min-Jung;Song, Woo-Young;Shin, Mi-Soo;Jang, Dong-Soon;Yun, Sang-June;Choi, Young-Chan;Lee, Gae-Goo
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.2
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    • pp.165-174
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    • 2010
  • The numerical modeling of a coal gasification reaction occurring in an entrained flow coal gasifier is presented in this study. The purposes of this study are to develop a reliable evaluation method of coal gasifier not only for the basic design but also further system operation optimization using a CFD(Computational Fluid Dynamics) method. The coal gasification reaction consists of a series of reaction processes such as water evaporation, coal devolatilization, heterogeneous char reactions, and coal-off gaseous reaction in two-phase, turbulent and radiation participating media. Both numerical and experimental studies are made for the 1.0 ton/day entrained flow coal gasifier installed in the Korea Institute of Energy Research (KIER). The comprehensive computer program in this study is made basically using commercial CFD program by implementing several subroutines necessary for gasification process, which include Eddy-Breakup model together with the harmonic mean approach for turbulent reaction. Further Lagrangian approach in particle trajectory is adopted with the consideration of turbulent effect caused by the non-linearity of drag force, etc. The program developed is successfully evaluated against experimental data such as profiles of temperature and gaseous species concentration together with the cold gas efficiency. Further intensive investigation has been made in terms of the size distribution of pulverized coal particle, the slurry concentration, and the design parameters of gasifier. These parameters considered in this study are compared and evaluated each other through the calculated syngas production rate and cold gas efficiency, appearing to directly affect gasification performance. Considering the complexity of entrained coal gasification, even if the results of this study looks physically reasonable and consistent in parametric study, more efforts of elaborating modeling together with the systematic evaluation against experimental data are necessary for the development of an reliable design tool using CFD method.