• Title/Summary/Keyword: Solid state reaction method

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Studies on the fabrication and properties of $La_ 0.7Sr_0.3MnO_3$cathode contact prepared by glycine-nitrate process and solid state reaction method for the high efficient solid oxide fuel cells applications 0.3/Mn $O_{3}$ (고효율 고체산화물 연료전지 개발을 위한 자발 착화 연소 합성법과 고상반응법에 의한 $La_ 0.7Sr_0.3MnO_3$ 양극재료 제조 및 물성에 관한 연구)

  • Shin, Woong-Shun;Park, In-Sik;Kim, Sun-Jae;Park, Sung
    • Electrical & Electronic Materials
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    • v.10 no.2
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    • pp.141-149
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    • 1997
  • L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ powders were prepared by both GNP(Glycine-Nitrate Process) and solid state reaction method in various of calcination temperature(800-1000.deg. C) and time in air. Also, L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ cathode contacts on YSZ(Yttria-Stabilized Zirconia) substrate were prepared by screen printing and sintering method as a function of sintering temperature(1100-1450.deg. C) in air. Sintering behaviors have been investigated by SEM(Scanning Electron Microscope) and porosity measurement. Compositional and structural characterization were carried out by X-ray diffractometer and ICP AES(Inductively Coupled Plasma-Atomic Emission Spectrometry) analysis. Electrical characterization was carried out by the electrical conductivity with linear 4 point probe method. As the calcination period increased in solid state reaction method, L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ phase increased. Although L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ single phase was obtained only for 48hrs at 1000.deg. C, in GNP method it was easy to get single and ultra-fine L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ powders with submicron particle size at 650.deg. C for 30min. The particle size and thickness of L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ cathode contact by solid state reaction method did not change during the heat treatment, while those by GNP method showed good sintering characteristics because initial powder size fabricated from GNP method is smaller than that fabricated from solid state reaction method. Based on enthalpy change from thermodynamic data and ICP-AES analysis, it was suggested to make cathode contact in composition of (L $a_{0.7}$S $r_{0.3}$)$_{0.91}$ Mn $O_{3}$ which have little second phase (L $a_{2}$Z $r_{2}$ $O_{7}$) for high efficient solid oxide fuel cells applications. As (L $a_{0.7}$S $r_{0.3}$)$_{0.91}$Mn $O_{3}$ cathode contact on YSZ substrate was sintering at 1250.deg. C the temperature that liquid phase sintering did not occur. It was possible to obtain proper cathode contacts with electrical conductivity of 150(S/cm) and porosity content of 30-40%.m) and porosity content of 30-40%.

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The SrLiAl3N4:Eu2+ Phosphor Synthesized by the Raw Material Model Obtained by DFT Calculations

  • Park, Woon Bae
    • Journal of the Korean Ceramic Society
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    • v.54 no.3
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    • pp.217-221
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    • 2017
  • Improvement studies of existing phosphors are needed for use in light emitting diodes (LEDs). Among the phosphors discovered recently, the SLA ($SrLiAl_3N_4:Eu^{2+}$) is a phosphor that has a narrow width. It is now known as a good red phosphor that meets the industry's needs for warm white (color temperature ranging from 2700 to 4000 K) and high CRI (> 80). However, SLA phosphors are obtained from difficult synthetic methods. All commercially available phosphors should be derived from the general solid state synthesis method. The phosphors produced by difficult synthetic methods will inevitably fall out of price competitiveness and will be scrapped. This study succeeded in synthesizing SLA ($SrLiAl_3N_4:Eu^{2+}$) phosphors by using a general solid phase synthesis method based on the reaction energy obtained from DFT calculations. As a result, we found an optimal solid state synthesis method for SLA phosphors.

Solid-State Ball-Mill Synthesis of Prussian Blue from Fe(II) and Cyanide Ions and the Influence of Reactants Ratio on the Products at Room Temperature

  • Youngjin Jeon
    • Journal of the Korean Chemical Society
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    • v.68 no.2
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    • pp.82-86
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    • 2024
  • This paper presents the solid-state synthesis of insoluble Prussian blue (Fe4[Fe(CN)6]3·xH2O, PB) in a ball mill, utilizing the fundamental components of PB. Solid-state synthesis offers several advantages, such as being solvent-free, quantitative, and easily scalable for industrial production. Traditionally, the solid-state synthesis of PB has been limited to the reaction between iron(II/III) ions and hexacyanoferrate(II/III) complex ions, essentially an extension of the solution-based coprecipitation method to solid-state reaction. Taking a bottom-up approach, a reaction is designed where the reactants consist of the basic building blocks of PB: Fe2+ ions and CN- ions. The reaction, with a molar ratio of Fe2+ and CN- corresponding to 1:2.8, yields PB, while a ratio of 1:6.6 results in a mixture of potassium hexacyanoferrate(II) (K4Fe(CN)6), potassium chloride (KCl), and potassium cyanide (KCN). This synthetic approach holds promise for environmentally friendly methods to synthesize multimetallic PB with maximum entropy in nearly quantitative yield.

Reaction Characterization of Y2Ba1CU1O5 Oxides by Solid State Reaction Method and Pyrophoric Synthesis Method (고상반응법과 발화합성법에 의한 Y2Ba1CU1O5 산화물의 반응특성)

  • Park, Jeong-Shik
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.772-777
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    • 1999
  • $Y_2Ba_1Cu_1O_5(Y211)$ powders were prepared by pyrophoric synthesis method and by solid state reaction method using $Y_2O_3(99.9%)$, $BaCO_3(99.9%)$, and CuO(99.9%) powders in both of these processes. The phase formation and reaction kinetics of $Y_2Ba_1Cu_1O_5$ powders have been studied using X-ray diffraction analysis(XRD) of samples at various heat treatment temperatures and reaction time. The reaction characterization suggested that the phase formation rate is mainly controlled by the particle size of Y211 powders. The activation energy(${\Delta}E_a$) of Y211 phase formation in this pyrophoric synthesis method was found to be 136.42 kJ/mol compared with 149.46 kJ/mol for that of solid state reaction method. These results data showed that the pyrophoric synthesis method is kineticaly more efficient than the solid state reaction method in this $Y_2Ba_1Cu_1O_5$ system.

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Microstructure Evolution of Solid State Reacted HAp/β-TCP Composite Powders by Post-Treatment Processing (후처리공정에 따른 고상반응 β-TCP/HAp 복합분체의 미세구조 변화)

  • 박영민;양태영;박상희;윤석영;박홍채
    • Journal of the Korean Ceramic Society
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    • v.41 no.8
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    • pp.582-587
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    • 2004
  • Biphasic Calcium Phosphate (BCP) consisted of hydroxyapatite (HAp) and $\beta$-tricalcium phosphate (P-TCP) has been prepared by solid state reaction. The size reduction of the resultant BCP agglomerate was carried out by reaction with hot water under atmospheric condition uld also under high pressure using an autoclave. The influence of processing conditions on the change of crystalline phase and composition, relative amount of constituent, specific surface area, and microstructure was investigated by means of XRD, FT-IR, BET method using a nitrogen adsorption and SEM.

Development of Click Chemistry in Polymerization and Applications of Click Polymer

  • Karim, Md. Anwarul
    • Rubber Technology
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    • v.13 no.1
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    • pp.1-9
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    • 2012
  • Click chemistry had enjoyed a wealthy decade after it was introduced by K.B.Sharpless and his co-worker on 2001. Since there is no optimized method for synthesis of click polymer, therefore, this paper introduced three click reaction methods such as catalyst, non-catalyst and azide-end capping for fluorene-based functional click polymers. The obtained polymers have reasonable molecular weight with narrow PDI. The polymers are thermally stable and almost emitted blue light emission. The synthesized fluorene-based functional click polymers were characterized to compare the effect of click reaction methods on polymer electro-optical properties as well as device performance on quasi-solid-state dye sensitized solar cells (DSSCs) applications. The DSSCs with configuration of $SnO_2:F/TiO_2/N719$ dye/quasi-solid-state electrolyte/Pt devices were fabricated using these click polymers as a solid-state electrolyte components. Among the devices, the catalyzed click polymer composed device exhibited a high power conversion efficiency of 4.62% under AM 1.5G illumination ($100mW/cm^2$).These click polymers are promising materials in device application and $Cu^I$-catalyst 1, 3-dipolar cycloaddition click reaction is an efficient synthetic methodology.

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Synthesis of Ultrafine LaAlO$_3$ Powders with Good Sinterability by Self-Sustaining Combustion Method Using (Glycine+Urea) Fuel ((Glycine+Urea) 혼합연료를 이요한 자발착화 연소반응법에 의한 우수한 소결성의 초미분체 LaAlO$_3$ 분말 합성)

  • Nam, H.D.;Choi, W.S.;Lee, B.H.;Park, S.
    • Journal of the Korean Ceramic Society
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    • v.36 no.2
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    • pp.203-209
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    • 1999
  • LaAlO3d single phase used as the butter layer on Si wafer for YBa2Cu3O7-$\delta$ superconductor application were prepared by solid state reaction method and by self-sustaining combustion process. The microstructure and crystallity of synthesiszed LaAlO3 powder studied using scanning electron microscope (SEM) and X-ray diffractometer(XRD), specific surface area and sintering characteristics fo powder were investigated by Brunauer-Emmett-Teller (BET) method and dilatometer respectively. In solid state reaction method, it is difficult to obtain LaAlO3 single phase up to 150$0^{\circ}C$ period. However, in self-sustaining combustion process, it is to easy to do it only $650^{\circ}C$. Based on the results of analysis of dilatometer it is easier to obtain high sintering density (98.87%) in self-sustaining combustion process than in the solid state reaction method. This reason is that the average particle size prepared by self-sustaining combustion process is nano crystal size and has high specific surface are value(56.54 $m^2$/g) compared with that by solid state reaction method. Also, LaAlO3 layer on the Si wafer has been achieved by screen printing and sintering method. Even though the sintering temperature is 130$0^{\circ}C$, the phenomena of silicon out diffusion in LaAlO3/Si interphase are not observed.

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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.

Solid-state metathetic synthesis of MWO4 (M=Zn, Co) particles assisted by microwave irradiation

  • Lim, Chang-Sung
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.6
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    • pp.295-300
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    • 2010
  • Metathetic route for the $MWO_4$ (M=Zn, Co) particles is a simple method of synthesis and a viable alternative method in a short time. $MWO_4$ (M=Zn, Co) particles were synthesized using solid-state metathetic (SSM) method with microwave irradiation. The $MWO_4$ (M=Zn, Co) particles were formed completely at $600^{\circ}C$ for 3 h. The crystallization process, thermal decomposition and morphology of the $MWO_4$(M= Zn, Co) particles were evaluated. The characteristics of the SSM reaction and the formation of a high lattice energy by-product NaCl were discussed.

Superconducting Properties of Ge Substitution for the Bi Site in the 2212 Phase of Bi-Sr-Ca-Cu-O Superconductors (Bi계 산화물 초전도체 2212상에 있어서 Bi 자리에 Ge 치환에 따른 초전도 특성)

  • 신재수;이민수;최봉수;송승용;송기영
    • Journal of the Korean Ceramic Society
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    • v.37 no.8
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    • pp.787-791
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    • 2000
  • Samples with the nominal composition, Bi2-xGexSr2CaCu2O8+$\delta$ (x=0, 0.1, 0.2, 0.3, 0.4, 0.5) were prepared by the solid-state reaction method. We have studied the effect of substitution Ge for Bi and investigated the superconducting properties by changing oxygen content with Ge substitution. It was found that temperature difference, ΔK, between TCon and TCzero was considerably smaller in the samples prepared by the intermediate pressing method than that in the samples by the solid-state reaction method. We found the solubility limit of Ge to the 80 K single phase was around x=0.3. Within the solubility limit, lattice constant c decreased with the increase of x. In the region of the 80K single phase, the onset critical temperature TCon increased and excess oxygen content decreased with increase of x.

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