• Title/Summary/Keyword: Solid-State Synthesis

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Synthesis and Characterization of (THF)3 Li(NC)CU(C6H3-2,6-Mes2)and Br(THF)2 Mg(C6H3-2,6-Trip2) (Mes = C6H2-2,4,6-Me3; Trip = C6H2-2,4,6-i-Pr3): The Structures of a Monomeric Lower-Order Lithi

  • Hwang, Cheong-Soo;Power, Philip P.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.5
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    • pp.605-609
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    • 2003
  • The lower-order lithium organocyanocuprate compound, (THF)₃Li(NC)Cu($C_6$H₃-2,6-Mes₂) (1), and the bulky terphenyl Grignard reagent, Br(THF)₂Mg($C_6$H₃-2,6-Trip₂) (2), have been synthesized and structurally characterized both in the solid state by single crystal x-ray crystallography and in solution by multi-nuclear NMR and IR spectroscopy. The compound (1) was isolated as a monomeric contact ion-pair in which the C (organic ipso)-Cu-CN-Li atoms are coordinated linearly. The lithium has a tetrahedral geometry as a result of solvation by three THF molecules. The compound (1) is the first example of fully characterized monomeric lower order lithium organocyanocuprate. The bulky Grignard reagent (2) was also isolated as a monomer in which the magnesium, solvated by two THF molecules, has a distorted tetrahedral geometry. The crystals of (1) possess triclinic symmetry with the space group $P{\={1}}$, Z = 2, with a = 12.456(3) Å, b = 12.508(3) Å, c = 13.904(3) Å, α = 99.81°, β = 103.72(3)°, and γ = 119.44(3)°. The crystals (2) have a monoclinic symmetry of space group $P2_{1/C}$, Z = 4, with a = 13.071(3) Å, b = 14.967(3) Å, c = 22.070(4) Å, and β = 98.95(3)°.

Preparation and Characterization of Black Zirconia Ceramics by Black Color Spinel Pigment (스피넬계 흑색 안료를 이용한 흑색 지르코니아 세라믹스의 제조 및 특성분석)

  • Lee, Kwang-Ho;Lee, Yong-Seok;Park, Joo-Seok;Lee, Byung-Ha
    • Journal of the Korean Ceramic Society
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    • v.45 no.4
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    • pp.214-219
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    • 2008
  • The zirconia ceramics are widely used because of their excellent mechanical properties. Recently, many researches to make a colored zirconia was achieved to satisfy the individual aesthetic requirements. In this study, the synthesis of black-color spinel-based inorganic pigments which are stable above $1400^{\circ}C$ and the fabrication of black-colored zirconia using the synthesized pigments are investigated. Inorganic pigments which have spinel structure and near black color were synthesized by a solid state reaction method using a $Fe_2O_3,\;Cr_2O_3$, CoO and NiO powder as a starting materials at $1600^{\circ}C$. Most of synthesized pigments were black colored spinel phases and single spinel phase was successfully synthesized at the composition range of $Cr_2O_3:25{\sim}35%,\;Fe_2O_3:45{\sim}55%$, CoO:20% and NiO:$6{\sim}10%$. The black-colored zirconia was fabricated at $1410^{\circ}C$ with the 5 wt% synthesized pigments and their properties were evaluated. The results showed that the strength value was more than 848 MPa, absorption rate was 0.1%, the brightness of color was $L^*:40{\sim}42$, the tone of color is $a^*:0.2{\sim}0.8$ and $b^*:-1.1{\sim}2.4$. As a result, the black-colored zirconia was suitable for a artificial jewelry or decoration zirconia goods.

Synthesis and Photoluminescence Properties of Blue Phosphor Y1-xBO3:Cex3+ (청색 형광체 Y1-xBO3:Cex3+의 합성과 발광 특성)

  • Cho, Shin-Ho
    • Journal of the Korean Vacuum Society
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    • v.20 no.3
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    • pp.176-181
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    • 2011
  • $Y_{1-x}BO_3:Ce_x^{3+}$ ceramic phosphors were synthesized with changing the concentration of $Ce^{3+}$ ion by using a solid-state reaction method. The crystal structure, surface morphology, and optical properties of the blue phosphors were investigated by using X-ray diffractometer (XRD), scanning electron microscopy, and photoluminescence and photoluminescence excitation spectrophotometry, respectively. The XRD results showed that the main peak of the phosphor powders occurs at (401)와 ($31\bar{2}$) planes. As for the optical properties, the excitation spectrum occurred at 243 nm and the value of blue emission intensity peaking at 469 nm reached the maximum when the concentration of $Ce^{3+}$ ion was 0.10 mol.

Growth and characterization of molecular beam epitaxy grown GaN thin films using single source precursor with ammonia

  • Chandrasekar, P.V.;Lim, Hyun-Chul;Chang, Dong-Mi;Ahn, Se-Yong;Kim, Chang-Gyoun;Kim, Do-Jin
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.174-174
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    • 2010
  • Gallium Nitride(GaN) attracts great attention due to their wide band gap energy (3.4eV), high thermal stability to the solid state lighting devices like LED, Laser diode, UV photo detector, spintronic devices, solar cells, sensors etc. Recently, researchers are interested in synthesis of polycrystalline and amorphous GaN which has also attracted towards optoelectronic device applications significantly. One of the alternatives to deposit GaN at low temperature is to use Single Source Molecular Percursor (SSP) which provides preformed Ga-N bonding. Moreover, our group succeeds in hybridization of SSP synthesized GaN with Single wall carbon nanotube which could be applicable in field emitting devices, hybrid LEDs and sensors. In this work, the GaN thin films were deposited on c-axis oriented sapphire substrate by MBE (Molecular Beam Epitaxy) using novel single source precursor of dimethyl gallium azido-tert-butylamine($Me_2Ga(N_3)NH_2C(CH_3)_3$) with additional source of ammonia. The surface morphology, structural and optical properties of GaN thin films were analyzed for the deposition in the temperature range of $600^{\circ}C$ to $750^{\circ}C$. Electrical properties of deposited thin films were carried out by four point probe technique and home made Hall effect measurement. The effect of ammonia on the crystallinity, microstructure and optical properties of as-deposited thin films are discussed briefly. The crystalline quality of GaN thin film was improved with substrate temperature as indicated by XRD rocking curve measurement. Photoluminescence measurement shows broad emission around 350nm-650nm which could be related to impurities or defects.

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Effect of BaF2 as a Flux in Solid State Synthesis of Y3Al5O12:Ce3+ (고상법을 이용한 Y3Al5O12:Ce3+의 제조에서 BaF2가 미치는 영향)

  • Won, Hyung-Seok;Hayk, Nersisyan;Won, Chang-Whan;Won, Hyung-Il
    • Korean Journal of Materials Research
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    • v.21 no.11
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    • pp.604-610
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    • 2011
  • The effect of $BaF_2$ flux in $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) formation was investigated. Phase transformation of $Y_3Al_5O_{12}$(YAG) was characterized by using XRD, SEM, and TEM-EDS, and it was revealed that the sequential formation of the $Y_4Al_2O_9$(YAM), $YAlO_3$(YAP) and $Y_3Al_5O_{12}$(YAG) in the temperature range of 1000-1500$^{\circ}C$. Single phase of YAG was revealed from 1300$^{\circ}C$. In order to find out the effect of $BaF_2$ flux, three modeling experiments between starting materials (1.5$Al_2O_3$-2.5$Y_2O_3$, $Y_2O_3$-$BaF_2$, and $Al_2O_3$-$BaF_2$) were done. These modeling experiments showed that the nucleation process occurs via the dissolution-precipitation mechanism, whereas the grain growth process is controlled via the liquid-phase diffusion route. YAG:Ce phosphor particles prepared using a proposed technique exhibit a spherical shape, high crystallinity, and an emission intensity. According to the experimental results conducted in this investigation, 5% of $BaF_2$ was the best concentration for physical, chemical and optical properties of $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) that is approximately 10-15% greater than that of commercial phosphor powder.

Study on Synthesis and Properties of Water-born Polyurethane (수분산성 폴리우레탄의 합성 및 물성에 관한 연구)

  • Cho, Ur-Ryong;Choi, Seo-Yoon
    • Elastomers and Composites
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    • v.40 no.4
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    • pp.249-257
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    • 2005
  • Polyurethane(PU) prepolymers were prepared from polyol and diisocyanate. Unionized PU prepolymers were synthesized from poly(propylene glycol)(PPG, MW: 1000), 2,2-bis (hydroxymethyl) propionic acid(DMPA), and isophorone diisocyanate(IPDI) by prepolymer syhthesizing process. After PU prepolymers were dispersed into water, the physical properties were investigated by changing the molar ratio of polyol and diisocyanate. The results showed a stable state with the best physical properties when the prepolymer was composed of PPG/DMPA with hard segment=40%, NCO%=3.43%, [NCO]: [OH]=1.5: 1.0 in molar ratio, and was dispersed into water with 30% solid content. PU prepolymers also were synthesized with various molar ratio of PPG and DMPA. Upon higher molar ratio of DMPA, particle size of polyurethane dispersion(PUD) gradually decreased. PU-prepolymers prepared from the various blocking agents represented characteristic initial deblocking temperatures that depended on the blocking agents, and the beginning of deblocking occured within 30 mins on all the blocking agents used.

The Oxidation of Fullerene[$C_{60}$] using Several Oxidants under Microwave Irradiation (마이크로파 조건에서 여러가지 산화제를 이용한 풀러렌[$C_{60}$의 산화반응)

  • Ko, Weon-Bae;Hwang, Sung-Ho;Ahn, Ju-Hyun
    • Elastomers and Composites
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    • v.40 no.1
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    • pp.45-52
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    • 2005
  • Synthesis or fullerene oxides[$C_{60}(O)_n$] ($n=1{\sim}4$ or n=1) by fullerene[$C_{60}$] and several oxidants such as 3-chloroperoxy benzoic acid, benzoyl peroxide, trichloroisocyanuric acid, and chromium(VI) oxide took place under microwave irradiation. The reactivity in solid state of fullerene[$C_{60}$] with various oxidants under same microwave rendition increased in order or 3- chloroperoxy benzoic acid > benzoyl peroxide > trichloroisocyanuric acid $\simeq$chromium(VI) oxide. The MALDI-TOF-MS, UV-visible spectra and HPLC analysis confirmed that the products of fullerene oxidation were [$C_{60}(O)_n$] ($n=1{\sim}4$ or n=1).

Transition Metal Complexes Derived From 2-hydroxy-4-(p-tolyldiazenyl)benzylidene)-2-(p-tolylamino)acetohydrazide Synthesis, Structural Characterization, and Biological Activities

  • Alhakimi, Ahmed N.;Shakdofa, Mohamad M.E.;Saeed, S. El-Sayed;Shakdofa, Adel M.E.;Al-Fakeh, Maged S.;Abdu, Ashwaq M.;Alhagri, Ibrahim A.
    • Journal of the Korean Chemical Society
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    • v.65 no.2
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    • pp.93-105
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    • 2021
  • Mononuclear Cu(II), Ni(II), Co(II), Mn(II), Zn(II), Fe(III), Ru(III), and UO2(II) complexes of 2-hydroxy-4-(p-tolyldiazenyl)benzylidene)-2-(p-tolylamino)acetohydrazide (H2L) were prepared by direct method. The ligand and its complexes were isolated in solid state and characterized by analytical techniques such as elemental and thermal analyses, molar conductance, magnetic susceptibility measurements and spectroscopic techniques such as UV-Visible, IR, 1H-NMR and 13C-NMR. The spectral data indicated that the ligand acted as neutral/monobasic bidentate or monobasic/dibasic tridentate ligand bonded to the metal ions through the oxygen atom of ketonic or enolic carbonyl group, azomethine nitrogen atom and deprotonated/protonated phenolic oxygen atom forming either tetragonally distorted octahedral or octahedral. Antimicrobial activities of the ligand and its complexes were evaluated against Escherichia coli, Bacillus subtilis and Aspergillus niger by well diffusion method. The results of antifungal activity showed that the Fe(III) complex (10) exhibited higher antifungal against Aspergillus niger than the other complexes. However, the results of antibacterial activity revealed that Cu(II) complex (4) is the most active against Escherichia coli while the Cu(II) complex (5) and Fe(III) complex (10) exhibited higher antibacterial effect on Bacillus subtilis than the other complexes.

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 $2.6{\times}10^{12}{\Omega}$.

Crystal Structures and Electrochemical Properties of LiNi1-xMgxO2 (0≤x≤0.1) for Cathode Materials of Secondary Lithium Batteries (리튬 이차전지의 양극 활물질 LiNi1-xMgxO2 (0≤x≤0.1)의 결정구조 및 전기화학적 특성)

  • Kim, Deok-Hyeong;Jeong, Yeon Uk
    • Korean Journal of Metals and Materials
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    • v.48 no.3
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    • pp.262-267
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    • 2010
  • $LiNi_{1-x}Mg_xO_2$(x=0, 0.025, 0.05, 0.075, 0.1) samples were synthesized by the solid-state reaction method. The crystal structure was analyzed by X-ray powder diffraction and Rietveld refinement. $LiNi_{1-x}Mg_xO_2$samples give single phases of hexagonal layered structures with a space group of R-3m. The calculated cation-anion distances and angles from the Rietveld refinement were changed with Mg contents in $LiNi_{1-x}Mg_xO_2$. The thicknesses of $NiO_2$ slabs were increased and the distances between the $NiO_2$ slabs were decreased with the increase in Mg contents in the samples. The electrical conductivities of sintered $LiNi_{1-x}Mg_xO_2$ samples were around $10^{-2}$ S/cm at room temperature. The electrochemical performances of $LiNi_{1-x}Mg_xO_2$were evaluated by coin cell test. Compared to $LiNiO_2$, $LiNi_{0.95}Mg_{0.05}O_2$ exhibited improved high-rate capability and cyclability due to the well-ordered layered structure by doping of Mg ion.