• 제목/요약/키워드: Solid-state reaction method

검색결과 379건 처리시간 0.027초

고효율 고체산화물 연료전지 개발을 위한 자발 착화 연소 합성법과 고상반응법에 의한 $La_ 0.7Sr_0.3MnO_3$ 양극재료 제조 및 물성에 관한 연구 (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 $O_{3}$)

  • 신웅선;박인식;김선재;박성
    • E2M - 전기 전자와 첨단 소재
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    • 제10권2호
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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
    • 한국세라믹학회지
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    • 제54권3호
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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
    • 대한화학회지
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    • 제68권2호
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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.

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

  • 박정식
    • 공업화학
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    • 제10권5호
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    • pp.772-777
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    • 1999
  • $Y_2Ba_1Cu_1O_5(Y211)$ 분말은 출발물질로서 $Y_2O_3(99.9%)$, $BaCO_3(99.9%)$, and CuO(99.9%) 분말을 사용하여 고상반응법과 발화합성법을 이용하여 제조하였다. $Y_2Ba_1Cu_1O_5(Y211)$ 분말에 대한 상형성과 반응속도는 열처리 온도와 반응시간에 따른 시료들을 X-선 회절분석을 이용하여 연구하였다. X-선 회절선으로부터 측정된 전화율($X_{211}$)과 반응특성으로부터 상 형성속도가 분말의 입자크기에 의해 지배되는 것을 알 수 있었다. 그리고 발화합성법으로 제조된 Y211상의 활성화에너지(${\Delta}E_a$)는 고상반응법에 의해 제조된 것의 149.46 kJ/mol과 비교할 때 136.42 kJ/mol을 나타내었다. $Y_2Ba_1Cu_1O_5$계에서의 활성화에너지 값은 발화합성법이 고상반응법보다 더욱 효율적인 방법임을 보였다.

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

  • 박영민;양태영;박상희;윤석영;박홍채
    • 한국세라믹학회지
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    • 제41권8호
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    • pp.582-587
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    • 2004
  • 수산화아파타이트(HAp) 및 P-인산3칼슘($\beta$-TCP)으로 구성되는 2상 인산칼슘염(BCP)을 고상반응법으로 합성하고, 이를 상압 및 autoclave를 이용한 고압에서 수열반응 시킴으로써 응집입자의 미세화를 시도하였다. 이 과정에서 일어나는 결정 상 및 화학조성, 구성상의 상대적인 양, 비표면적, 미세구조의 변화에 미치는 공정조건의 영향을 XRD, FT-IR, 질소흡착에 의한 BET법, SEM을 이용하여 검토하였다.

Development of Click Chemistry in Polymerization and Applications of Click Polymer

  • Karim, Md. Anwarul
    • 고무기술
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    • 제13권1호
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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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(Glycine+Urea) 혼합연료를 이요한 자발착화 연소반응법에 의한 우수한 소결성의 초미분체 LaAlO$_3$ 분말 합성 (Synthesis of Ultrafine LaAlO$_3$ Powders with Good Sinterability by Self-Sustaining Combustion Method Using (Glycine+Urea) Fuel)

  • 남희동;최우성;이병하;박성
    • 한국세라믹학회지
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    • 제36권2호
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    • pp.203-209
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    • 1999
  • Si 기판위에 Ba2YCu3O7-$\delta$ 고온초전도체를 응용하기 위해 요구되는 buffer층으로 유망한 재료인 LaAlO3 단일상 분말을 고상반응법과 자발착한 연소반응법으로 제조하였다. 제조된 LaAlO3 분말의 입자형태와 결정상태는 scanning electron microscope (SEM)과 X-ray diffractometer (XRD)를 이용하여 분석하였다. 분말의 비표면적과 소결특성은 각각 Brunauer-Emmett-Teller(BET) 방법과 dilatometer를 측정하였다. 고상반응법으로 LaAlO3 분말을 제조할 때에는 하소온도를 150$0^{\circ}C$까지 높게 하여도 단일상을 얻는 것이 어려웠으나 자발착한 연소반응법에 의한 분말제조는 $650^{\circ}C$의 저온에서 하소하여도 쉽게 얻을 수 있었다. Dilatometer 측정을 통하여 분석해 보면, 고상반응법에 의한 분말보다 자발착한 연소반응법에 의한 분말로 제조된 소결체가 고상반응법에 의한 소결체에 비해 1.4배나 큰 소멸밀도(98.87%)를 가졌다. 이렇게 소결밀도에서 큰 차이가 나는 것은 자발착한 연소방법에 의한 분말의 평균 입자크기가 nano crystal size이고 비표면적 값(56.54 $m^2$/g)이 매우 크기 때문이다. 두가지 방법으로 제조된 분말을 이용, LaAlO3 layer를 스크린 프린팅과 소결법으로 Si 기판상에 제조하였으며 자발착한 연소합성법으로 제조된 분말은 110$0^{\circ}C$에서 우수한 소결특성을 나타내었다.

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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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    • 제28권9호
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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
    • 한국결정성장학회지
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    • 제20권6호
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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.

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

  • 신재수;이민수;최봉수;송승용;송기영
    • 한국세라믹학회지
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    • 제37권8호
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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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