• Title/Summary/Keyword: Solid-State Synthesis

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Synthesis and Characterization of LSGM Solid Electrolyte for Solid Oxide Fuel Cell (연료전지용 LSGM 페로브스카이트계 전해질의 합성 및 특성 연구)

  • Seong, Young-Hoon;Jo, Seung-Hwan;Muralidharan, P.;Kim, Do-Kyung
    • Journal of the Korean Ceramic Society
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    • v.44 no.12
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    • pp.696-702
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    • 2007
  • The family of (Sr,Mg)-doped $LaGaO_3$ compounds, which exhibit high ionic conductivity at $600-800^{\circ}C$ over a wide range of oxygen partial pressure, appears to be promising as the electrolyte for intermediate temperature solid oxide fuel cells. Conventional synthesis routes of (Sr,Mg)-doped $LaGaO_3$ compounds based on solid state reaction have some problems such as the formation of impurity phases, long sintering time and Ga loss during high temperature sintering. Phase stability problem especially, the formation of additional phases at the grain boundary is detrimental to the electrical properties of the electrolyte. From this point of view, we focused to synthesize single phase (Sr,Mg)-doped $LaGaO_3$ electrolyte at the stage of powder synthesis and to apply relatively low heat-treatment temperature using novel synthesis route based on combustion method. The synthesized powder and sintered bulk electrolytes were characterized by XRD, TG-DTA, FT-IR and SEM. AC impedance spectroscopy was used to characterize the electrical transport properties of the electrolyte with the consideration of the contribution of the bulk lattice and grain boundary to the total conductivity. Finally, relationship between synthesis condition and electrical properties of the (Sr, Mg)-doped $LaGaO_3$ electrolytes was discussed with the consideration of phase analysis results.

Synthesis and Electrochemical Properties of Nanocrystalline LiFePO4 Obtained by Different Methods

  • Son, C.G.;Chang, D.R.;Kim, H.S.;Lee, Y.S.
    • Journal of Electrochemical Science and Technology
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    • v.2 no.2
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    • pp.103-109
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    • 2011
  • Nanocrystalline $LiFePO_4$ powders were prepared at 660-$670^{\circ}C$ in an Ar atmosphere using two different synthetic routes, solid-state and sol-gel. Both materials showed well-developed XRD patterns without any impurity peaks. Particles composed in the range of 200-300 nm from the solid-state method, and 50-100 nm from the sol-gel method, were confirmed through scanning electron microscopy and dynamic light scattering. The $LiFePO_4$ obtained by the sol-gel method offered a high discharge capacity (153 mAh/g) and stable discharge behavior, even at elevated temperatures (50 and $60^{\circ}C$), whereas poor electrochemical performance was observed from the solid-state method. Rate capability studies for sol gel-derived $LiFePO_4$ ranged from 0.2 to 30 C, which revealed excellent retention over 70 cycles with a 99.9% capacity.

Single-Step Solid-State Synthesis of CeMgAl11O19:Tb Phosphor

  • Park, Byoung-Kyu;Lee, Seoung-Soo;Kang, Jun-Kun;Byeon, Song-Ho
    • Bulletin of the Korean Chemical Society
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    • v.28 no.9
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    • pp.1467-1471
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    • 2007
  • The green-emitting CeMgAl11O19:Tb (CMAT) phosphor has been prepared at 1200 °C by the simple solid-state reaction using AlF3 as a self-flux. This preparation temperature is much lower than those (1500-1700 °C) for conventional solid-state reaction and spray pyrolysis method. In particular, the complete process to produce high-quality phosphor particles was carried out through the single-step heat treatment of the mixture of corresponding oxide-type metal sources. An addition of AlF3 as a self-flux significantly decreased the crystallization temperature of CMAT with plate-like shape. The particle morphology could be controlled from plate-like to spherical by using H3BO3 as an additional flux. Thus, an optimal morphology and luminescence characteristics of CMAT were achieved when both AlF3 and H3BO3 fluxes were simultaneously used. Compared with conventional solid-state process, which is accompanied by the calcination step(s), and other alternative liquid solution techniques such as sol-gel method and spray pyrolysis, no use of active precursors and liquid media that are harmful to the environment is a distinctive advantage for the industrial purpose.

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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Synthesis and characterization of Y2O3 : Eu3+ red nano phosphor powders using RF thermal plasma (RF 열플라즈마를 이용한 Y2O3:Eu3+ 적색 나노 형광체 분말 합성)

  • Lee, Seung-Yong;Koo, Sang-Man;Hwang, Kwang-Taek;Kim, Jin-Ho;Han, Kyu-Sung
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.25 no.6
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    • pp.272-279
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    • 2015
  • $Y_2O_3:Eu^{3+}$ is an excellent red-emitting phosphor, which has been widely used for display devices due to highly luminescent property and chemical stability. In this study, $Y_2O_3:Eu^{3+}$ red phosphors were prepared using the solid state reaction and RF thermal plasma synthesis. The particle size of $Y_2O_3:Eu^{3+}$ phosphors obtained by the solid state reaction varied from 10 to $20{\mu}m$, and 30~100 nanometer sized $Y_2O_3:Eu^{3+}$ particles were obtained from a liquid form of raw material through RF thermal plasma synthesis without an additional heat treatment. Photoluminescence measurements of the obtained $Y_2O_3:Eu^{3+}$ particles showed a red emission peak at 611 nm ($^5D_0{\rightarrow}^7F_2$). PL intensity of red nano phosphors prepared by RF thermal plasma synthesis was comparable to that of red phosphors prepared by the solid state reaction, indicating that nano-sized $Y_2O_3:Eu^{3+}$ red phosphors could be successfully synthesized using one-step process of RF thermal plasma.

Synthesis of Boron Nitride Nanotubes via inductively Coupled thermal Plasma process Catalyzed by Solid-state ammonium Chloride

  • Chang, Mi Se;Nam, Young Gyun;Yang, Sangsun;Kim, Kyung Tae;Yu, Ji Hun;Kim, Yong-Jin;Jeong, Jae Won
    • Journal of Powder Materials
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    • v.25 no.2
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    • pp.120-125
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    • 2018
  • Boron nitride nanotubes (BNNTs) are receiving great attention because of their unusual material properties, such as high thermal conductivity, mechanical strength, and electrical resistance. However, high-throughput and high-efficiency synthesis of BNNTs has been hindered due to the high boiling point of boron (${\sim}4000^{\circ}C$) and weak interaction between boron and nitrogen. Although, hydrogen-catalyzed plasma synthesis has shown potential for scalable synthesis of BNNTs, the direct use of $H_2$ gas as a precursor material is not strongly recommended, as it is extremely flammable. In the present study, BNNTs have been synthesized using radio-frequency inductively coupled thermal plasma (RF-ITP) catalyzed by solid-state ammonium chloride ($NH_4Cl$), a safe catalyst materials for BNNT synthesis. Similar to BNNTs synthesized from h-BN (hexagonal boron nitride) + $H_2$, successful fabrication of BNNTs synthesized from $h-BN+NH_4Cl$ is confirmed by their sheet-like properties, FE-SEM images, and XRD analysis. In addition, improved dispersion properties in aqueous solution are found in BNNTs synthesized from $h-BN+NH_4Cl$.

Synthesis of Lanthanides Doped $CaTiO_3$ Powder by the Combustion Process

  • Jung, Choong-Hwan;Park, Ji-Yeon;Lee, Min-Yong;Oh, Seok-Jin;Kim, Hwan-Young;Hong, Gye-Won
    • The Korean Journal of Ceramics
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    • v.6 no.1
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    • pp.47-52
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    • 2000
  • Lanthanides such as La, Gd and Ce have recognized as elements of high level radioactive wastes immobilized by forming solid solution with $CaTiO_3$. For easy forming solid solution between $CaTiO_3$and lanthanides, the combustion synthesis process was applied and the powder characteristics and sinterability were investigated. The proper selection of the type and the composition of fuels are important to get the crystalline solid solution of $CaTiO_3$and lanthanides. When glycine or the mixtures of urea and citric acid with stoichiometric composition was used as a fuel, the solid solution of $CaTiO_3$with $La_2O_3$or $Gd_2O_3$or $CeO_2$was produced very well by the combustion process. The combustion synthesized powder seemed to have a good sinterability with the linear shrinkage of more than 25% up to $1500^{\circ}C$, while that of the solid state reacted powder was less than 10% at the same condition.

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Synthesis and Characterisation of Mixed Conducting Perovskite Type Oxide and Its Electrochemical Application to Electrode Material for Solid Oxide Fuel Cell

  • Kim, Yu-Mi;Pyun, Su-Il;Lee, Gyoung-Ja;Kim, Ju-Sik
    • Journal of the Korean Electrochemical Society
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    • v.10 no.2
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    • pp.116-125
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    • 2007
  • This article is concerned with synthesis, characterisation and electrochemical application of the mixed conducting perovskite type oxide to electrode materials for solid oxide fuel cell. First, this review provides a comprehensive survey of the various synthetic methods such as solid state reaction, Pechini, glycine nitrate process and sol-gel methods for the preparation of perovskite type oxide powders. Subsequently, the electrical and microstructural properties of the mixed conducting oxides were discussed in detail. Finally, as electrochemical applications of the mixed conducting perovskite type oxides to electrode materials for solid oxide fuel cell, fundamentals of theoretical ac-impedance model for porous mixed conducting electrodes were introduced. Furthermore, the ac-impedance behaviour of porous and dense mixed conducting electrodes prepared by various synthetic methods was discussed.

Synthesis of Solid Electrolyte Nasicon by Solid State Reaction

  • Kim, Cheol-Jin;Chung, Jun-Ki;Lim, Sung-Ki;Rhee, Meung-Ho
    • The Korean Journal of Ceramics
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    • v.2 no.1
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    • pp.25-32
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    • 1996
  • Solid electroyte nasion was synthesized by the optimized solid state reaction minimizing the volume fraction of secondary $ZrO_2$ and glassy phases. To compensate for the evaporation of Na and P during heat-treatment, excess Na and P were added to the starting composition $Na_{1+x} Zr_2 Si_x P_{d-x} O_{12}$ (x=2.1). Phases pure nasicon comparable in volume fraction to the one obtaied from sol-gel process were synthesized after the reaction at $1100~1150^{\circ}C$,$ P_{O2}>=0.1-0.15 $$ZrO_2$ increased with the heat-treatment time due to the decomposition of nasicon phase and that of glassy phase increased as partial oxygen pressure decreased. The synthesized nasion showed a good electrical conductivity of $-1{\times}10^{-2}({\omega}{\cdot}cm)^{-1}$ at $350^{\circ}C$.

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Development of Synthesis Process for Ammonia Borane using NaBH4 as the Hydrogen Storage Materials (NaBH4를 이용한 암모니아 보란 수소 저장 소재 합성 공정 개발)

  • Choi, Ho Yun;Park, Sung Jin;Jung, Sung Jin;Baek, Jong Min;Song, Han Dock;Kim, Jong Soo;Lee, Kun Jong;Kim, Young Lae
    • Transactions of the Korean hydrogen and new energy society
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    • v.25 no.5
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    • pp.475-481
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    • 2014
  • Ammonia borane ($NH_3BH_3$), as a source material for energy generation and hydrogen storage, has attracted growing interest due to its high hydrogen content. We have investigated the synthesis of ammonia borane from sodium borohydride ($NaBH_4$) and ammonium chloride ($NH_4Cl$) utilizing a low-temperature process. From our results, we obtained a maximum synthetic yield of 98.2% of ammonia borane complex. The diammoniate diborane (DADB) was detected in about 5~10mol% with in the solid ammonia borane by solid-state $^{11}B$-NMR analysis. The synthesized solid ammonia borane products were studied to characterize hydrogen release upon thermal dehydrogenation.