• 제목/요약/키워드: Solid-state synthesis

검색결과 355건 처리시간 0.025초

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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    • 제24권5호
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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)°.

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

  • 이광호;이용석;박주석;이병하
    • 한국세라믹학회지
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    • 제45권4호
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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.

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

  • 조신호
    • 한국진공학회지
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    • 제20권3호
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    • pp.176-181
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    • 2011
  • $Y_{1-x}BO_3:Ce_x^{3+}$ 세라믹 청색 형광체를 고상 반응법을 사용하여 $Ce^{3+}$ 이온의 농도를 변화시키면서 합성하였다. 청색 형광체의 결정 구조, 표면 형상과 광학 특성은 각각 X-선 회절 장치(XRD), 주사전자현미경, 광여기 및 발광 분광기를 사용하여 측정하였다. XRD 결과로부터 합성된 모든 형광체 분말의 주 피크는 (401)와 ($31\bar{2}$)면에서 발생한 회절 신호이었다. 광학 특성의 경우에, $Ce^{3+}$ 이온의 농도비가 0.10 mol일 때 여기 스펙트럼은 243 nm에서 발생하였고, 469 nm에 피크를 갖는 최대의 청색 형광 스펙트럼이 관측되었다.

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
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2009년도 제38회 동계학술대회 초록집
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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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고상법을 이용한 Y3Al5O12:Ce3+의 제조에서 BaF2가 미치는 영향 (Effect of BaF2 as a Flux in Solid State Synthesis of Y3Al5O12:Ce3+)

  • 원형석;;원창환;원형일
    • 한국재료학회지
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    • 제21권11호
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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.

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

  • 조을룡;최서윤
    • Elastomers and Composites
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    • 제40권4호
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    • pp.249-257
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    • 2005
  • 폴리우레탄 프리폴리머들이 폴리올과 디이소시아네이트로부터 제조되었다. 이온화되지 않은 폴리우레탄 프리폴리머들은 폴리프로필렌 글리콜(PPG, MW:1000), 디메치롤 프로피온산(DMPA)과 이소포론 디이소시아네이트(IPDI)를 사용하여 합성되었다. 폴리올과 디이소시아네이트의 몰비를 변화시키면서 합성된 폴리우레탄 프리폴리머들은 물에 분산된 후 물성을 측정하였다. 실험결과는 프리폴리머가 하드세그먼트 40%, NCO 3.43%, [NCO]:[OH]=1.5:1.0의 조건에서 가장 안정한 분산액을 보여 주었고, 30%의 고형분으로 물에 분산되었다. 폴리우레탄 프리폴리머들은 또한 PPG와 DMPA의 몰비를 변화시키면서 합성되었다. DMPA의 몰비가 높을 때 폴리우레탄 수분산액의 입경은 감소하였다 3가지 종류의 말단기 차단제(blocking agent)를 사용하여 제조된 폴리우레탄 프리폴리머들은 사용된 차단제에 따라 각각 다른 초기 해리 온도를 나타내었고 3가지 종류의 차단제에 대한 해리의 시작은 모두 30분 안에 일어났다.

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

  • 고원배;황성호;안주현
    • Elastomers and Composites
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    • 제40권1호
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    • pp.45-52
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    • 2005
  • 풀러렌[$C_{60}$]은 3-chloroperoxy benzoic acid, benzoyl peroxide, trichloroisocyanuric acid, chromium(VI) oxide 등의 산화제를 사용하여 마이크로파 조건에서 반응시켜 풀러렌 산화물[$C_{60}(O)_n$] ($n=1{\sim}4$ or n=1)을 합성하였다. 동일한 마이크로파 조건에서 여러 가지 산화제와 풀러렌[$C_{60}$]의 고체상태 반응성은 3-chloroperoxy benzoic acid>benzoyl peroxide>trichloroisocyanuric acid$\simeq$chromium(VI) oxide 순으로 증가함을 나타냈다. MALDI-TOF-MS, UV-visible, 그리고 HPLC를 사용하여 분석한 결과 생성된 풀러렌 산화물은[$C_{60}(O)_n$] ($n=1{\sim}4$ or n=1)임을 알 수 있었다.

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.
    • 대한화학회지
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    • 제65권2호
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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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    • 제19권6호
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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 $2.6{\times}10^{12}{\Omega}$.

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

  • 김덕형;정연욱
    • 대한금속재료학회지
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    • 제48권3호
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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.