• Title/Summary/Keyword: Solid-state reaction

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Wet Chemical Preparation of Li-rich LiMn$_2$O$_4$ Spinel by Oxalate Precipitation (Oxalate 침전을 이용한 Li-과량 LiMn$_2$O$_4$ Spinel의 습식합성가 분말 특성)

  • 이병우;김세호
    • Journal of the Korean Ceramic Society
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    • v.36 no.7
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    • pp.698-704
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    • 1999
  • Li rich Li1+xMn2-xO4(x=0.07) spinel powders were prepared by an oxalate precipitation of wet chemical methods at temperature lower than $600^{\circ}C$. The FTIR results showed that the powders prepared at $600^{\circ}C$ had high degree of crystal quality comparing with the spinel powders prepared by solid state reaction at 75$0^{\circ}C$ which was the lowest synthesis temperature of the solid state reaction method. The particle size of powders prepared by the oxalate precipitation at $600^{\circ}C$ was smaller than 0.2${\mu}{\textrm}{m}$ and the specific surface area was 11.01 m2/g A heat treatment over 90$0^{\circ}C$ formed second phase in the precipitates. It was shown that there were phase transitions at temperatures. T1,T2 and T2. The transitions involved weight loss and gain during heating and cooling. The low temperature synthesis below $600^{\circ}C$ avoided the second phase formation and the prepared powders showed improved compositional and physical properties for secondary lithium battery applications.

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Carbon Dioxide Sorption Properties and Sintering Behavior of Lithium Zirconate Prepared by Solid-State Reaction (고상반응에 의하여 제조된 Li2ZrO3의 이산화탄소 흡수 및 소결 특성)

  • Woo, Sang-Kuk;Lee, Shi-Woo;Yu, Ji-Haeng
    • Journal of the Korean Ceramic Society
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    • v.43 no.5 s.288
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    • pp.309-314
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    • 2006
  • We synthesized lithium zirconate using solid-state reaction and analyzed thermal properties (TG/DTA) of starting materials and the synthesized one. When $Li_2ZrO_3$ powder was exposed to $CO_2$ environment at $500^{\circ}C$, 93% of the theoretical absorption weight was gained within 280 min with fairly high sorption rate. Almost all the absorbed $CO_2$ was generated by heating the sample to $800^{\circ}C$. We also investigated densification behavior of $Li_2ZrO_3$ under $CO_2$ environment. By sintering $Li_2ZrO_3$ at $760^{\circ}C$ using 2-step process, we obtained dense product, composed mainly of $Li_2ZrO_3\;and\;ZrO_2$, with relative density of 92%.

In Situ Crosslinked Ionic Gel Polymer Electrolytes for Dye Sensitized Solar Cells

  • Shim, Hyo-Jin;Kim, Dong-Wook;Lee, Chang-Jin;Kang, Yong-Ku;Suh, Dong-Hack
    • Macromolecular Research
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    • v.16 no.5
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    • pp.424-428
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    • 2008
  • We prepared an ionic gel polymer electrolyte for dye-sensitized solar cells (DSSCs) without leakage problem. Triiodide compound (BTDI) was synthesized by the reaction of benzene tricarbonyl trichloride with diethylene glycol monotosylate and subsequent substitution of tosylate by iodide using NaI. Bisimidazole was prepared by the reaction of imidazole with the triethylene glycol ditosylate under strongly basic condition provided by NaH. BTDI and bisimidazole dissolved in an ionic liquid were injected into the cells and permeated into the $TiO_2$ nanopores. In situ crosslinking was then carried out by heating to form a network structure of poly(imidazolium iodide), thereby converting the ionic liquid electrolytes to a gel or a quasi-solid state. A monomer (BTDI and bisimidazole) concentration in the electrolytes of as low as 30 wt% was sufficient to form a stable gel type electrolyte. The DSSCs based on the gel polymer electrolytes showed a power conversion efficiency of as high as 1.15% with a short circuit current density of $5.69\;mAcm^{-2}$, an open circuit voltage of 0.525 V, and a fill factor of 0.43.

Synthesis of One-dimensional Spinel LiMn2O4 Nanostructures as a Positive Electrode in Lithium Ion Battery

  • Lee, Hyun-Wook;Muralidharan, P.;Kim, Do-Kyung
    • Journal of the Korean Ceramic Society
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    • v.48 no.5
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    • pp.379-383
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    • 2011
  • This paper presents the synthesis of one-dimensional spinel $LiMn_2O_4$ nanostructures using a facile and scalable two-step process. $LiMn_2O_4$ nanorods with average diameter of 100 nm and length of 1.5 ${\mu}m$ have been prepared by solid-state lithiation of hydrothermally synthesized ${\beta}$-$MnO_2$ nanorods. $LiMn_2O_4$ nanowires with diameter of 10 nm and length of several micrometers have been fabricated via solid-state lithiation of ${\beta}$-$MnO_2$ nanowires. The precursors have been lithiated with LiOH and reaction temperature and pressure have been controlled. The complete structural transformation to cubic phase and the maintenance of 1-D nanostructure morphology have been evaluated by XRD, SEM, and TEM analysis. The size distribution of the spinel $LiMn_2O_4$ nanorods/wires has been similar to the $MnO_2$ precursors. By control of reaction pressure, cubic 1-D spinel $LiMn_2O_4$ nanostructures have been fabricated from tetragonal $MnO_2$ precursors even below $500^{\circ}C$.

Photoluminescence Properties of Green Phosphor Y1-xBO3:Tbx3+ Synthesized by Solid-state Reaction Method (고상 반응법으로 제조한 녹색 형광체 Y1-xBO3:Tbx3+의 형광 특성)

  • Cho, Shin-Ho
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.24 no.8
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    • pp.659-663
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    • 2011
  • [ $Y_{1-x}BO_3:Tb_x^{3+}$ ]ceramic phosphors were synthesized with changing the concentration of $Tb^{3+}$ at a sintering temperature of $1,100^{\circ}C$ and a reduction temperature of $950^{\circ}C$ by using a solid-state reaction method. The crystal structure, surface morphology, and photoluminescence properties of the phosphors were investigated as a function of $Tb^{3+}$ ion concentration by using XRD (x-ray diffractometer), scanning electron microscopy, and photoluminescence spectrophotometry, respectively. The XRD results showed that the main peak of the phosphor powders occurs at (101) plane. As for the photoluminescence properties, the excitation spectra showed the broad band centered at 306 nm and the emission intensity of the spectra peaked at 543 nm indicated a significant decrease as the concentration of $Tb^{3+}$ ion is increased.

Microwave Dielectric Properties of Low-temperature Sintered $MgCo_2(VO_4)_2$ Ceramics Synthesized by Sol-Gel process (졸-겔 공정에 의해 제조된 저온소결 $MgCo_2(VO_4)_2$ 세라믹스의 마이크로파 유전특성)

  • Lee, Ji-Hun;Bang, Jae-Cheol
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2006.06a
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    • pp.288-289
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    • 2006
  • We studied the effect of sol-gel processing and sintering temperature on the microwave properties of $MgCo_2(VO_4)_2$ system(MCV) which is applicable to LTCC(low-temperature cofired ceramics). The MCV was synthesized by sol-gel process using solution that contains precursor molecules for Mg, Co, and V. SEM analysis shows that the average particle size is ${\sim}1{\mu}m$ and size distribution is very uniform compared to the one prepared by conventional solid-state reaction process. Highly dense samples were obtained at the sintering temperature range of $750^{\circ}C{\sim}930^{\circ}C$. The maximum $Q{\times}f_0$ value of 55,700GHz, dielectric constant(${\varepsilon}_r$) of 10.41 and temperature coefficient(${\tau}_f$) of $-85ppm/^{\circ}C$ was obtained at the sintering temperature of $930^{\circ}C$. The superior microwave properties of sol-gel processed MCV relative to conventional solid-state reaction processed one is remarkable especially at lower sintering temperatures such as $750^{\circ}C$ and $800^{\circ}C$.

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Electrical Properties of ZnxMn3-xO4 Ceramics for Application as IR Detectors

  • Kim, Kyeong-Min;Lee, Sung-Gap;Lee, Dong-Jin
    • Transactions on Electrical and Electronic Materials
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    • v.17 no.4
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    • pp.227-230
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    • 2016
  • ZnxMn3-xO4 (0.95≤x≤1.20) specimens were prepared using a conventional solid state reaction method. All specimens were sintered in air at 1,200℃ for 12 h, cooled at a rate of 2℃/min to 800℃, and subsequently quenched to room temperature. We investigated the electrical properties of ZnxMn3-xO4 specimens with various amounts of ZnO for use as IR detectors. At a composition of x≥1.15, the ZnO phase precipitates beside the spinel structure. The electrical resistivity at room temperature, activation energy, responsivity, and detectivity of a Zn1.10Mn1.90O4 specimen are 653.2 kΩ-cm, 0.392 eV, 0.016 V/W, and 7.52×103 cmHz1/2/W, respectively.

Photoluminescence properties of Mn4+-activated Li2ZnSn2O6 red phosphors

  • Choi, Byoung Su;Lee, Dong Hwa;Ryu, Jeong Ho;Cho, Hyun
    • Journal of Ceramic Processing Research
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    • v.20 no.1
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    • pp.80-83
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    • 2019
  • The Mn4+-activated Li2ZnSn2O6 (LZSO:Mn4+) red phosphors were synthesized by the solid-state reaction at temperatures of 1100-1400 ℃ in air. The synthesized LZSO:Mn4+ phosphors were confirmed to have a single hexagonal LZSO phase without the presence of any secondary phase formed by the Mn4+ addition. With near UV and blue excitation, the LZSO:Mn4+ phosphors exhibited a double band deep-red emission peaked at ~658 nm and ~673 nm due to the 2E → 4A2 transition of Mn4+ ion. PL emission intensity showed a strong dependence on the Mn4+ doping concentration and the 0.3 mol% Mn4+-doped LZSO phosphor produced the strongest PL emission intensity. Photoluminescence emission intensity was also found to be dependent on the calcination temperature and the optimal calcination temperature for the LZSO:Mn4+ phosphors was determined to be 1200 ℃. Dynamic light scattering (DLS) and field-effect scanning electron microscopy (FE-SEM) analysis revealed that the 0.3 mol% Mn4+-doped LZSO phosphor particles have an irregularly round shape and an average particle size of ~1.46 ㎛.

Formation of Hydroxyl Radical from the Hydrogen Chemisorbed Silicon Surface by Incident Oxygen Atoms

  • Ree, Jong-Baik;Chang, Kyung-Soon;Kim, Yoo-Hang;Shin, Hyung-Kyu
    • Bulletin of the Korean Chemical Society
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    • v.24 no.7
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    • pp.986-992
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    • 2003
  • We have calculated the probability of the OH formation and energy deposit of the reaction exothermicity in the newly formed OH, particularly in its vibrational motion, in the gas-surface reaction O(g) + H(ad)/Si → OH(g) + Si on the basis of the collision-induced Eley-Rideal mechanism. The reaction probability of the OH formation increases linearly with initial excitation of the HSi vibration. The translational and vibrational motions share most of the energy when the H-Si vibration is initially in the ground state. But, when the initial excitation increases, the vibrational energy of OH rises accordingly, while the energies shared by other motions vary only slightly. The product vibrational excitation is significant and the population distribution is inverted. Flow of energy between the reaction zone and the solid has been incorporated in trajectory calculations. The amount of energy propagated into the solid is only a few percent of the available energy released in the OH formation.

Synthesis of the orange color pigment in the system of TiO2-SnO-ZnO by solid state reaction (고상반응법에 의한 TiO2-SnO-ZnO의 주황 안료 합성에 관한 연구)

  • Kim, Soomin;Kim, Ungsoo;Cho, Woo Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.5
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    • pp.181-187
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    • 2016
  • In this study, new composition of orange color pigment was developed by replacing formerly used lead and chromium with environment-friendly elements. $TiO_2-SnO-ZnO$ composite was synthesized using the solid state reaction under the reducing atmosphere with the LPG and air mixture gas. The synthesized pigments were characterized by spectrophotometer, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and X-ray Photoelectron Spectroscopy (XPS). The colorimetric analysis of pigments exhibited color values ranging from yellow to orange-red. Five different crystalline phases were formed after the heat treatment for 4 and 6 hours. The color of pigments was strongly influenced by the crystalline structure of $SnO_2$, having either cubic or tetragonal structure. The oxidation state study of elements revealed that the color of pigment is getting close to rYR with the increase of $Sn^{4+}$ ratio.