• Title/Summary/Keyword: Solid-State Synthesis

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Luminescent Characteristics and Synthesis of Y3Al5O12:Eu3+ Red Phosphors (Y3Al5O12:Eu3+ 적색 형광체의 제조와 발광특성)

  • Yu, Il
    • Korean Journal of Materials Research
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    • v.32 no.10
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    • pp.425-428
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    • 2022
  • In this study, Y3Al5O12:Eu3+ red phosphors were synthesized at different temperatures using a solid state reaction method. The crystal structures, surface and optical properties of the Y3Al5O12:Eu3+ red phosphors were investigated using X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), and photoluminescence (PL) analyses. From XRD results, the crystal structure of the Y3Al5O12:Eu3+ red phosphors was determined to be cubic. The maximum emission spectra were observed for the Y3Al5O12:Eu3+ red phosphor prepared by annealing for 4h at 1,700 ℃. The 565~590 nm photoluminescent spectra of the Y3Al5O12:Eu3+ red phosphors is associated with the 5D07F2 magnetic dipole transition of the Eu3+ ions. The intensity of the photoluminescent spectra in the red phosphors is more dominant for the magnetic dipole transition than the electric dipole transition with increasing annealing temperature. The International Commission on Illumination (CIE) coordinates of Y3Al5O12:Eu3+ red phosphors prepared by 1,700 ℃ annealing temperature are X = 0.5994, Y = 0.3647.

Synthesis and Comparative Analysis of Crystallite Size and Lattice Strain of Pb2Ba1.7Sr0.3Ca2Cu3O10+δ Superconductor

  • Hasan, Maher Abd Ali;Jasim, Kareem Ali;Miran, Hussein Ali Jan
    • Korean Journal of Materials Research
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    • v.32 no.2
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    • pp.66-71
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    • 2022
  • In this article, Pb2Ba1.7Sr0.3Ca2Cu3O10+δ superconductor material was synthesized using conventional solid-state reaction method. X-ray diffraction (XRD) analysis demonstrated one dominant phase 2223 and some impurities in the product powder. The strongest peaks in the XRD pattern were successfully indexed assuming a pseudo-tetragonal cell with lattice constants of a = 3.732, b = 3.733 and c = 14.75 Å for a Pb-Based compound. The crystallite size and lattice strain between the layers of the studied compound were estimated using several methods, namely the Scherrer, Williamson-Hall (W.H), size-strain plot (SSP) and Halder Wagner (H.W) approach. The values of crystallite size, calculated by Scherrer, W.H, SSP and H.W methods, were 89.4540774, 86.658638, 87.7555823 and 85.470086 Å, respectively. Moreover, the lattice strain values obtained by W.H, SSP and H.W methods were 0.0063240, 0.006325 and 0.006, respectively. It was noted that all crystallite size results are consistent; however, the best method is the size-strain plot because it gave a value of R2 approaching one. Furthermore, degree of crystallites was calculated and found to be 59.003321%. Resistivity analysis suggests zero-resistance, which is typical of superconducting materials at critical temperature. Four-probe technique was utilized to measure the critical temperature at onset Tc(onset), zero resistivity Tc(off set), and transition (width ΔT), corresponding to temperatures of 128 K, 116 K, and 12 K, respectively.

Synthesis and Analysis of the Impact of Partial Mercury Replacement with Lead on the Structural and Electrical Properties of the Hg1-xPbxBa2Ca2Cu3O8+δ Superconductor

  • Kareem Ali Jasim;Chaiar Abdeen Zaynel Saleh;Alyaa Hamid Ali Jassim
    • Korean Journal of Materials Research
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    • v.34 no.1
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    • pp.21-26
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    • 2024
  • In this investigation, samples of the chemical (Hg1-xPbxBa2Ca1.8Mg0.2Cu3O8+δ) were prepared utilizing a solid-state reaction technique with a range of lead concentrations (x = 0.0, 0.05, 0.10, and 0.20). Specimens were pressed at 8 tons per square centimeter and then prepared at 1,138 K in the furnace. The crystalline structure and surface topography of all samples were examined using X-ray diffraction (XRD) and atomic force microscopy (AFM). X-ray diffraction results showed that all of the prepared samples had a tetragonal crystal structure. Also, the results showed that when lead was partially replaced with mercury, an increase in the lead value impacted the phase ratio, and lattice parameter values. The AFM results likewise showed excellent crystalline consistency and remarkable homogeneity during processing. The electrical resistivity was calculated as a function of temperature, and the results showed that all samples had a contagious behavior, as the resistivity decreased with decreasing temperature. The critical temperature was calculated and found to change, from 102, 96, 107, and 119 K, when increasing the lead values in the samples from 0.0 to 0.05, 0.10, and 0.20, respectively.

Synthesis of (Ba0.5Sr0.5)0.99Co0.2Fe0.8O3-δ (BSCF) and the Electrochemical Performance of the BSCF/GDC(Buffer)/ScSZ ((Ba0.5Sr0.5)0.99Co0.2Fe0.8O3-δ(BSCF)의 합성 및 BSCF/GDC(Buffer)/ScSZ의 전기화학적 특성)

  • Lim, Yong-Ho;Hwang, Hae-Jin;Moon, Ji-Woong;Park, Sun-Min;Choi, Byung-Hyun;Lee, Mi-Jai
    • Journal of the Korean Ceramic Society
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    • v.43 no.6 s.289
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    • pp.369-375
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    • 2006
  • [ $(Ba_{0.5}Sr_{0.5})_{0.99}Co_{x}Fe_{1-x}O_{3-{\delta}}$ ] [x=0.8, 0.2](BSCF) powders were synthesized by a Glycine-Nitrate Process (GNP) and the electrochemical performance of the BSCF cathode on a scandia stabilized zirconia, $[(Sc_{2}O_3)_{0.11}(ZrO_2)_{0.89}]-1Al_{2}O_3$ was investigated. In order to prevent unfavorable solid-state reactions between the cathode and zirconia electrolyte, a GDC ($Gd_{0.1}Ce_{0.9}O_{2-{delta}}$) buffer layer was applied on ScSZ. The BSCF (x = 0.8) cathode formed on GDC(Buffer)/ScSZ(Disk) showed poor electrochemical property, because the BSCF cathode layer peeled off after the heat-treatment. On the other hand, there were no delamination or peel off between the BSCF and GDC buffer layer, and the BSCF (x = 0.2) cathode exhibited fairly good electrochemical performances. It was considered that the observed phenomenon was associated with the thermal expansion mismatch between the cathode and buffer layer. The ohmic resistance of the double layer cathode was slightly lower than that of the single layer BSCF cathode due to the incorporation of platinum particle into the BSCF second layer.

Synthesis and Photovoltaic Properties of Dendritic Photosensitizers containing Carbazole and Phenothiazine for Dye-sensitized Solar Cells (카바졸과 페노시아진을 이용한 염료감응형 태양전지의 염료 합성과 광적특성)

  • Kim, MyeongSeok;Jung, DaeYoung;Kim, JaeHong
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.89.1-89.1
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    • 2010
  • Since Gratzel and co-workers developed a new type of solar cell based on the nanocrystalline $TiO_2$ electrode, dye-sensitized solar cells (DSSCs) have attracted considerable attention on account of their high solar energy-to-conversion efficiencies (11%), their easy manufacturing process with low cost production compared to conventional p-n junction solar cells. The mechanism of DSSC is based on the injection of electrons from the photoexcited dye into the conduction band of nanocrystalline $TiO_2$. The oxidized dye is reduced by the hole injection process from either the hole counter or electrolyte. Thus, the electronic structures, such as HOMO, LUMO, and HOMO-LUMO gap, of dye molecule in DSSC are deeply related to the electron transfer by photoexcitation and redox potential. To date, high performance and good stability of DSSC based on Ru-dyes as a photosensitizer had been widely addressed in the literatures. DSSC with Ru-bipyridyl complexes (N3 and N719), and the black ruthenium dye have achieved power conversion efficiencies up to 11.2% and 10.4%, respectively. However, the Ru-dyes are facing the problem of manufacturing costs and environmental issues. In order to obtain even cheaper photosensitizers for DSSC, metal-free organic photosensitizers are strongly desired. Metal-free organic dyes offer superior molar extinction coefficients, low cost, and a diversity of molecular structures, compared to conventional Ru-dyes. Recently, novel photosensitizers such as coumarin, merocyanine, cyanine, indoline, hemicyanine, triphenylamine, dialkylaniline, bis(dimethylfluorenyl)-aminophenyl, phenothiazine, tetrahydroquinoline, and carbazole based dyes have achieved solar-to-electrical power conversion efficiencies up to 5-9%. On the other hand, organic dye molecules have large ${\pi}$-conjugated planner structures which would bring out strong molecular stacking in their solid-state and poor solubility in their media. It was well known that the molecular stacking of organic dyes could reduce the electron transfer pathway in opto-electronic devices, significantly. In this paper, we have studied on synthesis and characterization of dendritic organic dyes with different number of electron acceptor/anchoring moieties in the end of dendrimer. The photovoltaic performances and the incident photon-to-current (IPCE) of these dyes were measured to evaluate the effects of the dendritic strucuture on the open-circuit voltage and the short-circuit current.

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Synthesis and characterization of perovskite nano-sized (Pb, La)$TiO_3$ powder using mechano chemical process (기계화학공정을 이용한 Perovskite 구조의 (Pb, La)$TiO_3$ 나노 분말 합성 및 특성)

  • Lim, Bo-Ra-Mi;Yang, Jae-Kyo;Lee, Dong-Suk;Noh, Tae-Hyung;Seo, Jung-Hye;Lee, Youn-Seoung;Kim, Hee-Taik;Choa, Yong-Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.5
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    • pp.200-204
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    • 2008
  • Mechano Chemical Process (MCP) skips the calcinations steps at an intermediate temperature that is always required in the conventional solid-state reaction because forming phase from raw powder is activated by mechanical energy. In this study, we prepared (Pb, La)$TiO_3$ nanopowder with perovskite structure by only high energy MCP. Especially, the PLT nanopowder was synthesized without any thermal treatment using oxides, not salts as raw powder. This process is also very simple due to dry milling method, unnecessary to dry of powder. The oxide powder was milled up to 12 hr at intervals of an hour using MCP and the pure PLT phase of perovskite structure was formed after milling time of 3 hr. And the average particle size was 20 nm with narrow distribution after milling time of 3 hr from raw powder of several $\mu m$ with inhomogeneous distribution.

Effect of the pH of Pyrophoric Synthetic Solution on the Formation Kinetics of Y1Ba2Cu3O7-x Superconducting Phase (발화합성용액의 pH가 Y1Ba2Cu3O7-x 초전도상 생성 속도에 미치는 영향)

  • Park, J.S.;Kim, Y.S.;Yang, S.W.;Kim, C.Y.;Shin, H.S.
    • Applied Chemistry for Engineering
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    • v.9 no.2
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    • pp.165-171
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    • 1998
  • The $Y_1Ba_2Cu_3O_{7-x}$(123) superconductor powders were prepared by pyrophoric synthesis method(PSM) using $Y_2O_3$(99.9%), $BaCO_3$(99.9%), and CuO(99.9%) powders. The phase formation and reaction kinetics of 123 superconductor manufactured with powders prepared in various pHs of pyrophoric synthetic solution have been studied through the experiments at various heat treatment temperatures and times. Inductively coupled plasma(ICP) spectroscopy and scanning electron microscopy(SEM) measurements were performed to examine the composition and morphology of the sample. X-ray diffraction(XRD) analysis was done to determine phase formation and conversion ratio of Y-Ba-Cu-O systems. The 123 powder prepared at pH 7(${\pm}0.3$) yields the best result in terms of purity, homogeneity, and reactivity. The activation energies(${\Delta}E_a$) of 123 phase formation were found to be 191 kJ/mol and 230kJ/mol in solid state reaction method and pyrophoric synthesis method, respectively.

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Electrochemical Properties of Lithium Secondary Battery and the Synthesis of Spherical Li4Ti5O12 Powder by Using TiCl4 As a Starting Material (TiCl4를 출발원료로한 구형 Li4Ti5O12 분말합성 및 리튬이차 전지특성)

  • Choi, Byung-Hyun;Ji, Mi-Jung;Kwon, Yong-Jin;Kim, Eun-Kyung;Nahm, Sahn
    • Korean Journal of Materials Research
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    • v.20 no.12
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    • pp.669-675
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    • 2010
  • One of the greatest challenges for our society is providing powerful electrochemical energy conversion and storage devices. Rechargeable lithium-ion batteries and fuel cells are among the most promising candidates in terms of energy and power density. As the starting material, $TiCl_4{\cdot}YCl_3$ solution and dispersing agent (HCP) were mixed and synthesized using ammonia as the precipitation agent, in order to prepare the nano size Y doped spherical $TiO_2$ precursor. Then, the $Li_4Ti_5O_{12}$ was synthesized using solid state reaction method through the stoichiometric mixture of Y doped spherical $TiO_2$ precursor and LiOH. The Ti mole increased the concentration of the spherical particle size due to the addition of HPC with a similar particle size distribution in a well in which $Li_4Ti_5O_{12}$ spherical particles could be obtained. The optimal synthesis conditions and the molar ratio of the Ti 0.05 mol reaction at $50^{\circ}C$ for 30 minutes and at $850^{\circ}C$ for 6 hours heat treatment time were optimized. $Li_4Ti_5O_{12}$ was prepared by the above conditions as a working electrode after generating the Coin cell; then, electrochemical properties were evaluated when the voltage range of 1.5V was flat, the initial capacity was 141 mAh/g, and cycle retention rate was 86%; also, redox reactions between 1.5 and 1.7V, which arose from the insertion and deintercalation of 0.005 mole of Y doping is not a case of doping because the C-rate characteristics were significantly better.

Synthesis and Spectroscopic Characterization of Manganese(II), Iron(III) and Cobalt(III) Complexes of Macrocyclic Ligand. Potential of Cobalt(III) Complex in Biological Activity

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.
    • Journal of the Korean Chemical Society
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    • v.55 no.6
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    • pp.919-925
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    • 2011
  • A new series of manganese(II), iron(III) and cobalt(III) complexes of 14-membered macrocyclic ligand, (3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane-1,8-diamine) have been prepared and characterized by elemental analyses, IR, UV-VIS, $^1H$- and $^{13}C$- NMR spectra, magnetic susceptibilities, conductivities, and ESR measurements. Molar conductance measurements in DMF solution indicate that the complexes are electrolytes. The ESR spectrum for cobalt(III) complex in $CD_3OD+10%D_2O$ after exposure to $^{60}Co-{\gamma}$-rays at 77 K using a 0.2217 M rad $h^{-1}$ vicrad source showed $g_{\perp}$ > $g_{\parallel}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_z2$ orbital with covalent bond character. In this case, the ligand hyperfine tensors are nearly collinear with ${\gamma}$-tensors, so there is no major tendency to bend. Therefore, little extra delocalization via the ring lobe of the $dz^2$ orbital occurs. However, the ESR spectrum in solid state after exposure to $^{60}Co-{\gamma}$-rays at 77 K showed $g_{\parallel}$ > $g_{\perp}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_x2_{-y}2$ ground state as the resulting spectrum contains a large number of randomly oriented molecules provided that, the principle directions of g and A tensors. Manganese (II) complex 2, $[H_{12}LMn]Cl_4.2H_2O$, showed six isotropic lines characteristic to an unpaired electron interacting with a nucleus of spin 5/2, however, iron(III) complex 3, $[H_{12}LFe]Cl_5.H_2O$, showed spectrum of a high spin $^{57}Fe$ (I=1/2), $d^5$ configuration. The geometry of these complexes was supported by elemental analyses, IR, electronic and ESR spectral studies. Complex 1 showed exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Synthesis, Characterization and ESR Studies of New Copper(II) Complexes of Vicinal Oxime Ligands (Vicinal Oxime 리간드의 새로운 구리(II) 착물에 대한 합성, 특성 및 ESR 연구)

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.603-611
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    • 2011
  • Ethoxylacetyl oxime ligands [HL, (1) and $H_2L^1$, (3)] react with copper(II) acetate monohydrate yield octahedral and square planar complexes, respectively. The complexes have been postulated due to elemental analyses, IR, UVVis. spectra, magnetic susceptibility, conductivity and ESR spectra. Molar conductance of the complexes in DMF indicates a non-ionic character. The ESR spectra of [$(L)_2Cu(H_2O)_2$], (2) complex at room temperature and 77K are characteristic of an axial symmetry ($d_{x2-y2}$) with covalent bond character and have a large line width typical of dipolar interactions. However, [$(L^1)Cu$], (4) complex in the solid state showed spectra of marked broadening and loss of hyperfine splitting confirming spinexchange interactions between the copper(II) sites. The spectrum of the doped copper(II) complex at room temperature showed super-hyperfine splitting from coordinated nitrogen atoms and it has an axial type ($d_{x2-y2}$) with covalent bond character and an essentially square-planar arrangement around the copper(II) ion. The spectrum of [$(L^1)Cu$], (4) in frozen methanol at 77K was characteristic of the triplet state of a dimer species and the distance found between the two copper(II) centers was calculated and is equal to 4.8 ${\AA}$.