• Title/Summary/Keyword: Sub-structure synthesis method

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Synthesis of α-oximinoketones, Precursor of CO2 Reduction Macrocyclic Coenzyme F430 Model Complexes

  • Kim, Gilhoon;Won, Hoshik
    • Journal of the Korean Magnetic Resonance Society
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    • v.21 no.4
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    • pp.139-144
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    • 2017
  • Ni(II) containing coenzyme F430 catalyzes the reduction of $CO_2$ in methanogen. Macrocyclic Ni(II) complexes with N,O shiff bases have been received a great attention since metal ions play an important role in the catalysis of reduction. The reducing power of metal complexes are supposed to be dependent on oxidoreduction state of metal ion and structural properties of macrocyclic ring moiety that can enhance electrochemical properties in catalytic process. Six different ${\alpha}$-oximinoketone compounds, precursor of macrocyclic ligands used in $CO_2$ reduction coenzyme F430 model complexes, were synthesized with yields over 90% and characterized by NMR. The molecular geometries of ${\alpha}$-oximinoketone analogues were fully optimized at Beck's-three-parameter hybrid (B3LYP) method in density functional theory (DFT) method with $6-31+G^*$ basis set using the ab initio program. In order to understand molecular planarity and substitutional effects that may enhance reducing power of metal ion are studied by computing the structure-dependent $^{13}C$-NMR chemical shift and comparing with experimental results.

Hydrothermal Synthesis of Ultra-fine SrAl2O4:Eu Powders and Investigation of their Photoluminescent Characteristics (수열합성법에 의한 SrAl2O4:Eu 초미세 분말 합성공정 및 형광 특성)

  • 박우식;김선재;김정식
    • Journal of the Korean Ceramic Society
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    • v.41 no.5
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    • pp.370-374
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    • 2004
  • Sr$_{l-x}$Ba$_{x}$Al$_2$O$_4$:Eu (x = 0, 0.1, 0.2, and 0.3 mol) phosphor was synthesized by the hydrothermal method and its properties of photoluminescence and long-afterglow were investigated. The mixtures of Sr(NO$_3$)$_2$, Al(NO$_3$)$_3$9$H_2O$, and Eu(NO$_3$)$_3$$.$6$H_2O$ salts dissolved in distilled water, after controlling their pH by NH$_4$OH solution, put into an Autoclave reactor with high temperature and pressure to react. Such synthesized SrAl$_2$O$_4$:Eu powders showed homogeneous and ultra-fine particles of sub-micron size. In order to have the photoluminescence characteristic, powders were heat treated at 1100 -140$0^{\circ}C$ for 2 h in Ar/H$_2$ reduction atmosphere. Photoluminescence spectra showed a excitation along the wide wavelength of 250 ∼ 450 nm, and broaden emission with maxima peak at 520 nm. Also, it showed a good long afterglow with decaying over 1000 sec after excitation illumination for 10 min. In addition, the microstructure and crystal structure of SrAl$_2$O$_4$:Eu powders were investigated by an SEM and XRD, respectively.

Synthesis and Characterization of TiO2/CuS Nanocomposite Fibers as a Visible Light-Driven Photocatalyst

  • An, HyeLan;Kang, Leeseung;Ahn, Hyo-Jin;Choa, Yong-Ho;Lee, Chan Gi
    • Journal of the Korean Ceramic Society
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    • v.55 no.3
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    • pp.267-274
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    • 2018
  • $TiO_2/CuS$ nanocomposites were fabricated by precipitation of nanosized CuS via sonochemical method on electrospun $TiO_2$ nanofibers, and their structure, chemical bonding states, optical properties, and photocatalytic activity were investigated. In the $TiO_2/CuS$ nanocomposite, the position of the conduction band for CuS was at a more negative than that of TiO; meanwhile, the position of the valence band for CuS was more positive than those for TiO, indicating a heterojunction structure belonging to type-II band alignment. Photocatalytic activity, measured by decomposition of methylene blue under visible-light irradiation (${\lambda}$ > 400 nm) for the $TiO_2/CuS$ nanocomposite, showed a value of 85.94% at 653 nm, which represented an improvement of 52% compared to that for single $TiO_2$ nanofiber (44.97% at 653 nm). Consequently, the photocatalyst with $TiO_2/CuS$ nanocomposite had excellent photocatalytic activity for methylene blue under visible-light irradiation, which could be explained by the formation of a heterojunction structure and improvement of the surface reaction by increase in surface area.

Improvement of Electrochemical Performance of LiFePO4 by Carbon Coating and Morphology Control into Porous Structure (LiFePO4/C의 carbon coating 방법 및 다공성 구조 형성에 의한 전기화학적 특성 개선)

  • Kong, Ki Chun;Ju, Jeh Beck
    • Journal of the Korean Electrochemical Society
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    • v.17 no.4
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    • pp.229-236
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    • 2014
  • In this study, the method to improve the electrochemical performance of $LiFePO_4$ by carbon coating and morphology control into porous structure was studied. The synthesis of $LiFePO_4$ was done by coprecipitation method by two step procedure. In the first step $FePO_4$ precursor was synthesized by coprecipitation method, followed by impregnation of lithium into the precursor at $750^{\circ}C$. The carbon coating was done by both physical and chemical coating processes. Using the physical coating process, the amount of coating layer was 6% and the capacity achieved was 125 mAh/g. In case of chemical coating process, the active material delivered 130~140 mAh/g, which is about 40% improvement of delivered capacity compared to uncoated $LiFePO_4$. For the morphology control into porous structure, we added nano particles of $Al_2O_3$ or $SiO_2$ into the active materials and formed the nanocomposite of ($Al_2O_3$ or $SiO_2$)/$LiFePO_4$. Between them, $SiO_2/LiFePO_4$ porous nanocomposite showed larger capacity of 132 mAh/g.

Synthesis and characterization of LiMn1.5Ni0.5O4 powders using polymerization complex method (착체중합법을 이용한 LiMn1.5Ni0.5O4 분말합성 및 특성평가)

  • Sin, Jae-Ho;Kim, Jin-Ho;Hwang, Hae-Jin;Kim, Ung-Soo;Cho, Woo-Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.22 no.4
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    • pp.194-199
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    • 2012
  • The $LiMn_{1.5}Ni_{0.5}O_4$, substituting a part of Mn with Ni in the $LiMn_2O_4$, the spinel structure has good charge-discharge cycle stability and high discharge capacity at 4.7 V. In this study $LiMn_{1.5}Ni_{0.5}O_4$ powders were synthesized by polymerization complex method. The effect on the characteristics of synthesized $LiMn_{1.5}Ni_{0.5}O_4$ powders was studied with citric acid (CA) : metal ion (ME) molar ratio (5 : 1, 10 : 1, 15 : 1, 30 : 1) and calcination temperature ($500{\sim}900^{\circ}C$). Single phase of $LiMn_{1.5}Ni_{0.5}O_4$ was observed from XRD analysis on the powders calcined at low ($500^{\circ}C$) and high temperatures ($900^{\circ}C$). The crystalline size and crystallinity increased with calcination temperature. At low calcination temperature the particle size decreased and specific surface area increased as the CA molar ratio increased. On the other hand, high particle growth rate at high calcination temperature interfered the particle size reduction and specific surface area increase induced by the increase of CA molar ratio.

Synthesis of Prussian Blue Analogue and Magnetic and Adsorption Characteristics of MnFe2O4 (프러시안 블루 유사체의 합성 및 MnFe2O4의 자성과 흡착 특성)

  • Lee, Hye-In;Kang, Kuk-Hyoun;Lee, Dong-Kyu
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.1
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    • pp.67-74
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    • 2016
  • The Prussian Blue Analogue(PBA) has three dimensional structure and the metal - organic framework material, and it has a variety configurations depending on the type of organic ligands. PBA has been receving an attention in the fields of biosensors, optical, catalytic, and hydrogen storage device. Also, it is an environmental friendly substance with a chemical stability. In addition, PBA is widely used in the filed of adsorption art since we can adjust the size of the fine pores. In this study, we synthesized $Mn_3[Fe(CN)_6]_2$, an organometallic framework chains by using a hydrothermal synthesis method. We used $K_4[Fe(CN)_6]$ and $MnCl_2$ as precursors. We also produced a manganese iron oxide, by baking the synthesized material. The effect of the size and shape of the particles was examined by controling pH of the precursor solution, the molar concentration of the precursor, and reaction time as the experimental variables. Synthesized absorbent was analyzed by XRD, SEM, FT-IR, UV-Vis, and TG / DTA to evaluate the adsorption properties of several dyes.

Oxidation behavior of (Mo1-xWx)Si2 high-temperature heating elements (초고온용 발열체 (Mo1-xWx)Si2의 산화거동에 대한 연구)

  • Lee, Sung-Chul;Myung, Jae-ha;Kim, Yong-Nam;Jeon, Minseok;Lee, Dong-won;Oh, Jong-Min;Kim, Bae-Yeon
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.30 no.5
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    • pp.200-207
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    • 2020
  • MoSi2, (Mo1/2W1/2)Si2, and WSi2 powders were synthesized by self-propagating high-temperature synthesis (SHS) method. The synthesized powders were heat-treated at 500, 1,000, 1,200, 1,300, 1,400, 1,500 and 1,600℃ in ambient atmosphere. Oxidation of Mo-W silicide powder was found at low temperature of 500℃. XRD structure analysis and DTA/TG data showed that MoO3 was formed with 500℃ heat treatment for 1 hour, and that it was α-cristobalite phase that was formed with 1200℃ heat treatment, not α-quartz phase which is commonly found and stable at room temperature. Existence of W accelerated decomposition at both low and high temperature. Fully sintered MoSi2 and (Mo1/2W1/2)Si2 specimen did not show decomposition or weight loss by oxidation, with 1 hour heat treatment at either low or high temperature. Notably, it was difficult to sinter WSi2 because of oxidation reaction at low temperature.

Induction Heating of Cylinderical MoSi2-based Susceptor (실린더형 MoSi2계 발열체의 유도가열 적용)

  • Lee, Sung-Chul;Kim, Yo Han;Myung, Jae-ha;Kim, Bae-Yeon
    • Korean Chemical Engineering Research
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    • v.57 no.4
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    • pp.553-558
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    • 2019
  • In present study, the cylindrical susceptor by the slip casting method was designed to apply high-temperature induction heating by using $(Mo,W)Si_2$ ceramics. $MoSi_2$-based materials were synthesized by SHS (Self-propagating High-temperature Synthesis) method. The phase and crystal structure of $MoSi_2$-based materials were confirmed by XRD analysis. The shape of cylindrical mold was synthesized for various thickness by using the slip casting method. Finally, the susceptor for induction heating was processed by sintering and heat treatment to form $SiO_2$ layer, which was confirmed on the surface of susceptor by SEM/EDS analysis. To evaluate the heating performance of $(Mo,W)Si_2$ cylinder susceptor, we measured the maximum surface temperature and heating rate in comparison with the rod heating element under constantly applied power. The induction heating of the $(Mo,W)Si_2$ cylinder showed excellent heating performance, reaches the maximum temperature of $1457^{\circ}C$, with the average heating rate of $19^{\circ}C/s$ at 2 kW

Synthesis and Characterization of Nanosized of Spinel LiMn2O4 via Sol-gel and Freeze Drying Methods

  • Seyedahmadian, Masoud;Houshyarazar, Shadi;Amirshaghaghi, Ahmad
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.622-628
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    • 2013
  • Nanocrystalline spinel lithium manganese oxide ($LiMn_2O_4$) powders with narrow-size-distribution, pure-phase particles, and high crystallinity with an average crystallite size of about 70 nm were synthesized at $600^{\circ}C$ for 6 h in air by freeze drying method. Spinel $LiMn_2O_4$ is also prepared by sol-gel using citric acid as a chelating agent. The influence of different parameters such as pH conditions, solvent, molar ratio of citric acid to total metal ions, calcination temperature, starting material on the structure, morphology and purity of this oxide was investigated. The results of sol-gel method show that pure $LiMn_2O_4$ with average crystallite size of about 130 nm can be produced from nitrate salts as starting materials at $800^{\circ}C$ for 6 h in air. The optimum pH and molar ratio of chelating agent to total metal ions are $4{\leq}pH{\leq}6$ and 1.0, respectively. A possible mechanism on the formation of the nanocrystallines synthesized by sol-gel was also discussed. At the end a comparison of the differences between two methods was made on the basis of x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) tests.

Dielectric properties and microstructures of (CaxSr1-x)ZrO3 ceramics

  • Li, Yu-De;Chen, Jian-Ming;Lee, Ying-Chieh
    • Journal of Ceramic Processing Research
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    • v.19 no.6
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    • pp.461-466
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    • 2018
  • The effects of Ca/Sr ratio and the sintering temperature on the properties of $(Ca_xSr_{(1-x)})ZrO_3$ (CSZ) ceramics were investigated in this study. CSZ ceramics were prepared using solid-state reaction process, which were sintered in air at temperatures ranging from $1350^{\circ}C$ to $1450^{\circ}C$. Their structures were characterized by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM). The change in Ca/Sr ratio significantly affected the crystalline phase and the dielectric properties of the $(Ca_xSr_{(1-x)})ZrO_3$ ceramics. The secondary phase, $Ca_{0.15}Zr_{0.85}O_{1.85}$, was observed and increased correspondingly with the rising of sintering temperatures. In order to understand the effects of secondary phase on the dielectric properties of CSZ ceramics, the $Ca_{0.15}Zr_{0.85}O_{1.85}$ phase was prepared individually using solidstate method. The $Ca_{0.15}Zr_{0.85}O_{1.85}$ ceramics sintered at $1500^{\circ}C$ for 2 hours possessed a dielectric constant (${\varepsilon}_r$) of 21.7, a dielectric loss ($tan{\delta}$) of $49.510^{-4}$ and an Insulation Resistance (IR) of $2.1{\times}10^{10}{\Omega}$. The ($Ca_{0.7}Sr_{0.3})ZrO_3$ ceramics exhibited the best dielectric properties, with a permittivity of 29, a dielectric loss ($tan{\delta}$) of $2.7{\times}10^{-4}$, and an Insulation Resistance (IR) of $2.6{\times}10^{12}{\Omega}$.