• Title/Summary/Keyword: Solid state synthesis

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Study on synthesis of Schiff base and its basic characteristics (Schiff base의 합성과 그의 기초적 물성에 관한 연구)

  • Shin, Dong-Gyu;Kwon, Oh-Kwan;Lim, Sung-Taek;Kim, Young-Kwan;Nam, Ki-Dae;Sohn, Byoung-Chung
    • Journal of the Korean Applied Science and Technology
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    • v.15 no.4
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    • pp.57-62
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    • 1998
  • In this study, a new conducting materials, namely, a Schiff base (polymeric azomethine) was synthesized from 2,6-diamino-N-docosyl pyridinium bromide and terephthalaldehyde to obtain a soluble and fusible conducting polymer. The synthesized Schiff base structure was analyzed by using UV/vis absorption spectrophotometer, FT-IR spectrometer and $^1H$-NMR spectrometer. It was found that the Schiff base was successfully synthesized and soluble in carbon tetrachloride$(CC^{14})$, its Langmuir-Blodgett film was easily fabricated, and its surface pressure was determined to be 30mN/m for solid state by measuring ${\pi}$-A isotherm.

Synthesis and Characterization of Layered Perovskite $La_{1+x}Sr_{2-x}Mn_2O_7$ Phases (층상구조형 Perovskite $La_{1+x}Sr_{2-x}Mn_2O_7$ 상의 합성 및 특성연구)

  • 송민석;서상일;이재열
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 1998.11a
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    • pp.271-274
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    • 1998
  • Metallic ferromagnet LA$_{1-x}$ Sr$_{x}$MnO$_3$ has received considerable attentions because of its metallic conductivity and giant magnetic resistivity. It is generally believed that layered perovskite SrO(LA$_{1-x}$ Sr$_{x}$MnO$_3$)$_{n}$ phase is insulating and shows no metallic transition. But recent report revealed that some single crystal SrO(LA$_{1-x}$ Sr$_{x}$MnO$_3$)$_{n}$ phase showed MR effect. In this study, layered perovskite SrO(LA$_{1-x}$ Sr$_{x}$MnO$_3$)$_2$ Phases were synthesized by solid state reaction at 140$0^{\circ}C$ in air atmosphere, for wide range of x and their phases were confirmed by X-ray diffraction. Electrical and magnetic properties were measured down to 10K and the possibility of MR effects was investigated.as investigated.

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Sonochemical Synthesis of $PbMoO_4$ Nanoparticles and Evaluation of its Photocatalytic Activity

  • Uresti, Diana B. Hernandez;De la Cruz, Azael Martinez;Martinez, Leticia M. Torres;Lee, Soo-Wohn
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.49.2-49.2
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    • 2011
  • $PbMoO_4$ nanoparticles were successfully obtained in the presence of ethylene glycol (EG) with the assistance of a prolonged sonication process. The nanoparticles were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS) and adsorption-desorption $N_2$ isotherms (BET). The catalyst prepared sonochemically showed higher photocatalytic activity than $PbMoO_4$ prepared by solid-state reaction in the degradation reactions of rhodamine B (rhB), indigo carmine (IC), orange G (OG), and methyl orange (MO) under UV-Vis light radiation. In order to elucidate aspects of the degradation mechanism of the organic dyes, some experimental variables were modified such as pH, $O_2$ level in solution, and radiation source. In general, the photocatalytic activity for the degradation of organic dyes followed the sequence IC>OG>rhB>MO.

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Synthesis of Lu2.94Ce0.06MgAl3SiO12 phosphor and its photoluminescent properties

  • Lee, Jung-Il;Kim, Tae Wan;Shin, Ji Young;Ryu, Jeong Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.25 no.3
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    • pp.121-126
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    • 2015
  • A novel $Ce^{3+}$ doped $Lu_3MgAl_3SiO_{12}$ phosphor ($Lu_{2.94}Ce_{0.06}MgAl_3SiO_{12}$) was successfully synthesized by a conventional solid-state reaction at $1450^{\circ}C$ for 5 h. The crystal structure of the synthesized phosphor powder was characterized by X-ray diffraction and Rietveld refinement. The prepared phosphor powder showed a broad peak at 550 nm, and the temperature dependence on photoluminescence properties of the prepared $Lu_{2.94}Ce_{0.06}MgAl_3SiO_{12}$ phosphor was investigated from 300 to 525 K. The activation energy for thermal quenching was determined by Arrhenius fitting. The experimental results clearly indicate that prepared $Lu_{2.94}Ce_{0.06}MgAl_3SiO_{12}$ phosphor has great potential for a down-conversion yellow phosphor in white light-emitting diodes.

Photoelectrochemical Water Splitting on a Delafossite CuGaO2 Semiconductor Electrode

  • Lee, Myeongsoon;Kim, Don;Yoon, Yong Tae;Kim, Yeong Il
    • Bulletin of the Korean Chemical Society
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    • v.35 no.11
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    • pp.3261-3266
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    • 2014
  • A pellet of polycrystalline $CuGaO_2$ with a delafossite structure was prepared from $Ga_2O_3$ and CuO by high-temperature solid-state synthesis. The $CuGaO_2$ pellet was a p-type semiconductor for which the electrical conductivity, carrier density, carrier mobility and Seebeck coefficient were $5.34{\times}10^{-2}{\Omega}^{-1}cm^{-1}$, $3.5{\times}10^{20}cm^{-3}$, $9.5{\times}10^{-4}cm^2V^{-1}s^{-1}$ at room temperature, and $+360{\mu}V/K$, respectively. It also exhibited two optical transitions at about 2.7 and 3.6 eV. The photoelectrochemical properties of the $CuGaO_2$ pellet electrode were investigated in aqueous electrolyte solutions. The flat-band potential of this electrode, determined using a Mott-Schottky plot, was +0.18 V vs SCE at pH 4.8 and followed the Nernst equation with respect to pH. Under UV light illumination, a cathodic photocurrent developed, and molecular hydrogen simultaneously evolved on the surface of the electrode due to the direct reduction of water without deposition of any metal catalyst.

Synthesis and Performance of Li2MnSiO4 as an Electrode Material for Hybrid Supercapacitor Applications

  • Karthikeyan, K.;Amaresh, S.;Son, J.N.;Lee, Y.S.
    • Journal of Electrochemical Science and Technology
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    • v.3 no.2
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    • pp.72-79
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    • 2012
  • $Li_2MnSiO_4$ was synthesized using the solid-state method under an Ar atmosphere at three different calcination temperatures (900, 950, and $1000^{\circ}C$). The optimization of the carbon coating was also carried out using various molar concentrations of adipic acid as the carbon source. The XRD pattern confirmed that the resulting $Li_2MnSiO_4$ particles exhibited an orthorhombic structure with a $Pmn2_1$ space group. Cyclic voltammetry was utilized to investigate the capacitive behavior of $Li_2MnSiO_4$ along with activated carbon (AC) in a hybrid supercapacitor with a two-electrode cell configuration. The $Li_2MnSiO_4$/AC cell exhibited a high discharge capacitance and energy density of $43.2Fg^{-1}$ and $54Whkg^{-1}$, respectively, at $1.0mAcm^{-2}$. The $Li_2MnSiO_4$/AC hybrid supercapacitor exhibited an excellent cycling stability over 1000 measured cycles with coulombic efficiency over > 99 %. Electrochemical impedance spectroscopy was conducted to corroborate the results that were obtained and described.

Preparation of Proton-Conducting Gd-Doped Barium Cerate by Oxalate Coprecipitation Method

  • Yong Sung Choi;Soo Man Sim
    • The Korean Journal of Ceramics
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    • v.4 no.3
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    • pp.213-221
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    • 1998
  • $BaCe_{0.9}Gd_{0.1_O_{2.95}$ powder was synthesized by oxalate coprecipitation method. Precipitate with a stoichimetric ratio of the cations was prepared by adding a mixture of Ba, Ce and Gd nitrate solution to an oxalic acid solution at pH 4. Reaction between the constituent oxides to form a perovskite phase was initiated at $800^{\circ}C$ and a single phase $BaCe_{0.9}Gd_{0.1_O_{2.95}$ powder having good sinterability was obtained after calcination at $1000^{\circ}C$. Sintering green compacts of this powder for 6 h showed a considerable densification to start at $1100^{\circ}C$ and resulted in 93% and 97% relative densities at $1300^{\circ}$ and at $1450^{\circ}C$, respectively. Whereas the power compacts prepared by solid state reaction had lower relative densities, 78% at $1300^{\circ}$and 90% at $1450^{\circ}C$. Fine particles of $CeO_2$ second phase were observed in the surface of the sintered compacts. This was attributed to the evaporation of BaO from the surface that had been exposed during thermal etching.

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Synthesis and Characterization of (Cr, Fe)-doped Y2O3-Al2O3 Red Pigments ((Cr, Fe)-doped Y2O3-Al2O3계 붉은 안료의 합성과 특성)

  • Shin, Kyung-Hyun;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.46 no.4
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    • pp.350-356
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    • 2009
  • Perovskite codoped with chromium and iron have been studied. Samples with $YAl_{0.96}(Cr_{0.04-x}Fe_x)O_3$(x=0.01, 0.02, 0.03, 0.04) were prepared by solid state reaction at $1450^{\circ}C$ for 6 h and were characterized by XRD, FT-IR, Raman spectroscopy, SEM and UV-vis spectrophotometer. The color of the synthesized pigments were from red to dark brown(in bulk). Up to 0.02 mole $Fe_2O_3$ for substituting $Cr_2O_3$ development of color in lime-glaze gives good red color but as increasing amount of $Fe_2O_3$ and decreasing $Cr_2O_3$ proportionally produce from brownish red to brown. Increasing $Fe_2O_3$ amount lead to weaken crystal field relatively due to have smaller ionic radius than $Cr_2O_3$ ionic one. The UV-vis peaks were shifted to lower wavelength.

Synthesis of new Pb-based layered cuprates in (Pb,S)(Sr,La)CuOz compounds

  • Kim, Jin;Lee, Ho Keun
    • Progress in Superconductivity and Cryogenics
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    • v.20 no.3
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    • pp.1-4
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    • 2018
  • The effect of sulfate substitution on the formation of (Pb,S)-1201 type phase was investigated. Polycrystalline samples with nominal compositions of $(Pb_{0.5}B_{0.5-x}S_x)(Sr_{2-y}La_y)CuO_z$, (x = 0 - 0.5, y = 0.7 - 1.0) and $(Pb_{0.5}S_{0.5})(Sr_{2-y}La_y)CuO_z$ (y = 0.5 - 1.0) were prepared by using a solid-state reaction method. The samples were characterized by powder X-ray diffraction (XRD) and resistivity measurements. XRD data revealed that almost-single (Pb,S)-1201 phase samples could be obtained for x = 0.5 and y = 0.9-1.0, judging from the similar results of the XRD patterns between the (Pb,S)-1201 and (Pb,B)-1201 phases. Each of the samples has a crystal structure with tetragonal symmetry. The sample with x = 0.5 and y = 0.9 is found to show an onset of resistivity dropping at over 23 K and zero resistivity at 12 K.

Synthesis and Characterization of Transition Metal(Ⅱ) Complexes with Tridentate Schiff Base in DMF Solution (DMF용액에서 세자리 Schiff Base를 가진 전이금속(II) 착물들의 합성과 구조결정)

  • Oh, Jeong Geun;Choi, Yong Kook
    • Journal of the Korean Chemical Society
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    • v.43 no.5
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    • pp.511-516
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    • 1999
  • Shiff Base ligand such as [NOIPH] have been synthesized from 2-hydroxy-1-naphthaldehyde and arometic amine. Co(II), Ni(II), and Cu(II) complexes from the reaction metal salts with Tridentate Schiff Base [NOIPH] were sythesized. The ligand and metal(II) complexes were characterized by the elementary analysis, IR, UV-Vis, NMR spectra, and thermogravimetric analysis. Metal(II) complexes in solid state have been shown that the mole raio of Schiff base [NOIPH] as $N_2O$ type to Metal(II) is 2:1 and the metal(II) complexes of $N_2O$ ligand type were four-coordinated configuration.

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