• Title/Summary/Keyword: Solution-phase chemical reduction

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Synthesis of Sub-Micron 2SnO·(H2O) Powders Using Chemical Reduction Process and Thermal Calcination (화학적 합성법을 이용한 마이크론 이하급 2SnO·(H2O) 분말의 합성과 하소 특성)

  • Chee, Sang-Soo;Lee, Jong-Hyun
    • Korean Journal of Materials Research
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    • v.23 no.11
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    • pp.631-637
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    • 2013
  • Synthesis of sub-micron $2SnO{\cdot}(H_2O)$ powders by chemical reduction process was performed at room temperature as function of viscosity of methanol solution and molecular weight of PVP (polyvinylpyrrolidone). Tin(II) 2-ethylhexanoate and sodium borohydride were used as the tin precursor and the reducing agent, respectively. Simultaneous calcination and sintering processes were additionally performed by heating the $2SnO{\cdot}(H_2O)$ powders. In the synthesis of the $2SnO{\cdot}(H_2O)$ powders, it was possible to control the powder size using different combinations of the methanol solution viscosity and the PVP molecular weight. The molecular weight of PVP particularly influenced the size of the synthesized $2SnO{\cdot}(H_2O)$ powders. A holding time of 1 hr in air at $500^{\circ}C$ sufficiently transformed the $2SnO{\cdot}(H_2O)$ into $SnO_2$ phase; however, most of the PVP (molecular weight: 1,300,000) surface-capped powders decomposed and was removed after heating for 1 h at $700^{\circ}C$. Hence, heating for 1 h at $500^{\circ}C$ made a porous $SnO_2$ film containing residual PVP, whereas dense $SnO_2$ films with no significant amount of PVP formed after heating for 1 h at $700^{\circ}C$.

Preparation of Nano-sized Pt Powders by Solution-phase Reduction (액상환원법(液相還元法)에 의한 백금(白金) 나노분말(粉末) 제조(製造))

  • Kim, Chul-Joo;Yoon, Ho-Sung;Cho, Sung-Wook;Sohn, Jung-Soo
    • Resources Recycling
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    • v.16 no.5
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    • pp.36-40
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    • 2007
  • Platinum plays an important role in many applications because of its extraordinary physical and chemical properties. All these applications require the use of platinum in the finely divided state. Therefore the preparation of platinum nanoparticles by reducing platinum-surfactant salt with reducing agent in the solution was investigated in this study. The net interaction between C14TABr and $H_2[PtCl_6]$ in aqueous solution results in the formation of $[C14TA]_2[PtCl_6]$. The concentration of C14TABr and the concentration of $H_2[PtCl_6]$ has to be above cmc and 0.32 mM, respectively in order to obtain complex-micelle aggregation for mono dispersed Pt particles. Pt particle size increases with increasing $H_2[PtCl_6]$ and C14TABr concentration. And the shape of Pt particles was well controlled with increasing surfactant concentration.

Growth methanism of ZnO nanowire syntheized by carbo-thermal reduction method (열적 탄소 환원법으로 제조된 ZnO 나노와이어의 성장 메커니즘)

  • 손광석;김현정;박병호;김동규;조형균;김인수
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.11a
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    • pp.173-173
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    • 2003
  • Nanowire와 nanorod 같은 1차원의 반도체 재료는 디멘젼과 크기와 물리적 특성과의 관계 등을 연구하는데 중요한 역할을 하며 laser ablation, arc discharge, chemical vapor depostion, vapor phase transport Process와 solution등의 방법으로 성공적으로 합성되었다. ZnO 는 3.37eV의 넓은 밴드갭과 다른 넓은 밴드갭 재료에 비해 높은 exciton bindng energy (60meV)를 가지며 UV LED, laser diode에 적용하기 유리하고 최근 디스플레나 나노 광전소자로서의 가능성 이 대두되면서 최근 이에 관한 연구가 증가하고 있다. 본 연구에서는 열적탄소환원법(carbothermal reduction process)으로 ZnO와 graphite 분말을 1:1 중량비로 혼합한 분말을 90$0^{\circ}C$, 100$0^{\circ}C$에서 air 분위기에서 20분간 반응 후 로 내에서 냉각 하였다. 직경 이 50nm-1000nm, 길이가 수 미크론인 내부 결함이 전혀 없는 육각형 단결정의 nanowire가 합성되었고 XRD, FE-SEM과 TEM으로 조성 및 형상, 내부구조를 분석하였다. 합성된 ZnO nanowire는 직경 이 변하는 부분에서 성장방향으로의 계단을 형성하였고 이는 layer by layer 방법으로 nanowire가 성장한다는 것을 나타낸다.

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A Study on the Synthesis of Co-ferrite by High-energy Ball Milling and Thermal Reduction Characteristics (고 에너지 볼 밀링을 통한 Co-ferrite 제조 및 열적 환원에 대한 연구)

  • Cho, M.S.;Kim, W.J.;Kim, C.H.;Kang, K.S.;Kim, Y.H.;Park, C.S.
    • Transactions of the Korean hydrogen and new energy society
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    • v.17 no.3
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    • pp.309-316
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    • 2006
  • Co-ferrite was synthesized by HEBM (High Energy Ball Milling) with a stoichiometric (Co/Fe=0.5/2.5) mixture of CoO and $Fe_2O_3$ powders. The effect of milling time on the phase transformation of the mixture was investigated by XRD. Mono-phase solid solution of Co-ferrite, which was milled for 4 h and then calcined at $900^{\circ}C$ in the Ar atmosphere, was confirmed by XRD analysis. The composition and thermal reduction behavior of Co-ferrite were analyzed by TGA and XRF. As a result, oxygen deficient Co-ferrite was synthesized by HEBM and the weight decrease of the Co-ferrite, which was oxidized at $600^{\circ}C$ for 10h by $H_2O$ vapor, was 2.41 wt% during thermal reduction at $1300^{\circ}C$.

Fabrication of Nano-sized Metal Dispersed Magnesia Based Composites and Related Mechanical and Magnetic Properties

  • Choa, Yong-Ho;Tadachika Nakayama;Tohru Sekino;Koichi Niihara
    • The Korean Journal of Ceramics
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    • v.5 no.4
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    • pp.395-399
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    • 1999
  • MgO/metal nanocomposite powder mixtures were prepared by solution chemical processes to obtain suitable structure for ceramic/metal nanocomposites. Nickel or cobalt nitrate, as a source of metal dispersion, was dissolved into alcohol and mixed with magnesia powder. After calcined in air, these powders were reduced by hydrogen. Densified nanocomposites were successively obtained by Pulse Electric Current Sintering (PECS) process. The dispersed metal partical size depended on temperature and time in calcination and reduction processes. The phase analyses in the synthesized powders as a functioni of temperature were tracked using a dynamic high temperature X-ray diffractioni (HTXRD) system. Phase and crystallite size analyses were done using X-ray diffractioni and TEM. The MgO/metal nanocomposites were successfully fabricated, and ferromagnetic responses with enhanced coercive force were also investigated for these composites.

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A STUDY ON THE LYOTROPIC LIQUID CRYSTALLINE COPOLYAMIDE

  • Lee, Chul-Joo;Min, Byoung-Gill;Son, Tea-Won;Yoon, Han-Sik
    • Proceedings of the Korean Fiber Society Conference
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    • 1987.06b
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    • pp.12-12
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    • 1987
  • To improve the fibrillation phenomenon and processibili to of poly(p-phenyleneterephthalamide) (PPD-T) , a P/E copolyamide was prepared by introducing 4,4'-ethylene dianiline (EDA) into rigid chain backbone. The effects of semi-flexible segment on the liquid crystalline properties were investigated. The EDA, used as a comonomer, was prepared by catalylitic reduction of p,p'-dinitrophenyl , obtained by oxidative coupling of p,p'-dinitrotoluene. Various high molecular weight PIE copolyamides were prepared by low temperature solution polycondensation of terephthaloyl chloride (TPC) with various mixtures of p-phenylene diamine (PPD) and EOA. The PfE copolyamides were completely dissolved in 100% svlfuric acid, and the phase transition of P/E copolyamide-sulfuric acid systems was examined in teams of concentration and temperature. Over the chemical compositions, PIE=911, 812, and 713, solutions of anisotropic single phase were acquired. In particular, the two mixing ratios, 911 and 812, gave a good anisotropic spinning dope.

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Electrochemical Properties of Activated Polyacrylonitrile/pitch Carbon Fibers Produced Using Electrospinning

  • Kim, Bo-Hye;Bui, Nhu-Ngoc;Yang, Kap-Seung;dela Cruz, Marilou E.;Ferraris, John P.
    • Bulletin of the Korean Chemical Society
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    • v.30 no.9
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    • pp.1967-1972
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    • 2009
  • The electrospinnability of pitch was improved by blending in a solution of polyacrylonitrile (PAN) resulting in the reduction of the average fiber diameter from 2000 to 750 nm. Activated carbon fibers (ACFs) derived by stabilization, carbonization and steam activation at 700, 800, and 900 ${^{\circ}C}$ of the PAN/pitch electrospun fibers for 60 min were investigated as electrodes for supercapacitors. The Brunauer, Emmett, Teller (BET) specific surface area ranged from 732 to 1877 $m^2g^{-1}$ and the specific capacitance from 75.5 to 143.5 $Fg^{-1}$, depending on the activation conditions. Electrodes from the electrospun web activated at 900 ${^{\circ}C}$ exhibited a particularly quick response showing a high frequency of 5.5 Hz at a phase angle of ‒$45^o$ of the impedance spectroscopy.

Speciation of Chromium in Water Samples with Homogeneous Liquid-Liquid Extraction and Determination by Flame Atomic Absorption Spectrometry

  • Abkenar, Shiva Dehghan;Hosseini, Morteza;Dahaghin, Zohreh;Salavati-Niasari, Masoud;Jamali, Mohammad Reza
    • Bulletin of the Korean Chemical Society
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    • v.31 no.10
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    • pp.2813-2818
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    • 2010
  • A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion ($TBA^+$)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a $100\;{\mu}L$ micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = $1.0{\times}10^{-4}\;M$, [$TBA^+$] = $2.0{\times}10^{-2}\;M$, [$CHCl_3$] = $100.0\;{\mu}L$ and [$ClO_4$] = $2.0{\times}10{-2}\;M$, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results.

Absorption Characteristics of Carbon Dioxide by Water-lean Diethylenetriamine Absorbents Mixed with Physical Solvents (물리 흡수제를 포함한 디에틸렌트리아민(Diethylenetriamine) 저수계 흡수제에서의 이산화탄소 흡수 특성)

  • Lee, Hwa Young;Seok, Chang Hwan;You, Jong-Kyun;Hong, Yeon Ki
    • Clean Technology
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    • v.24 no.1
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    • pp.50-54
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    • 2018
  • In this work, N-methyl-2-pyrrolidone (NMP) was added into diethylenetriamine (DETA) aqueous solution for high $CO_2$ loading via phase splitting of absorbents during $CO_2$ absorption. Immiscible two phases were formed in the range of more than 30 wt% of NMP in 2 M DETA + NMP + water absorbents because of low solubility of DETA-carbamate in NMP solution. As the composition of NMP in the absorbents increased, the difference of $CO_2$ loading between each phase increased and the volume of bottom phase decreased. In $CO_2$ absorption in packed column by 2 M DETA + NMP + water absorbents, the absorption rate decreased in the range of more than 40 wt% of NMP. It is due to the increasing of mass transfer resistance in liquid film of absorbents at the high concentration of NMP. DETA + NMP + water absorbent is expected as the promising one for reducing the regeneration energy of absorbents according to volume reduction of $CO_2-rich$ phase.

Recent Development of Carbon Dioxide Conversion Technology (이산화탄소 전환 기술의 현황)

  • Choi, Ji-Na;Chang, Tae-Sun;Kim, Beom-Sik
    • Clean Technology
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    • v.18 no.3
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    • pp.229-249
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    • 2012
  • At present, global warming and depletion of fossil fuels have been one of the big issues which should be solved for sustainable development in the future. CCS (carbon capture and sequestration) technology as the post $CO_2$ reduction technology has been considered as a promising solution for global warming due to increased carbon emission. However, the environmental and ecological effects of CCS have drawn concerns. There are needs for noble post reduction technology. More recently, CCU (carbon capture and utilization) Technology, which emphasizes transforming carbon dioxide into value-added chemicals rather than storing it, has been attracted attentions in terms of preventing global warming and recycling the renewable carbon source. In this paper, various technologies developed for carbon dioxide conversion both in gas and liquid phase have been reviewed. For the thermochemical catalysis in gas phase, the development of the catalytic system which can be performed at mild condition and the separation and purification technology with low energy supply is required. For the photochemical conversion in liquid phase, efficient photosensitizers and photocatalysts should be developed, and the photoelectrochemical systems which can utilize solar and electric energy simultaneously are also in development for more efficient carbon dioxide conversion. The energy needed in CCU must be renewable or unutilized one. CCU will be a key connection technology between renewable energy and bio industry development.