• Title/Summary/Keyword: Pechini process

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Low Temperature Synthesis of BaCeO3 Nano Powders by the Citrate Process (Citrate Process를 이용한 BaCeO3 나노 분말의 저온 합성)

  • Lee, Dong-Wook;Won, Jong-Han;Joo, Kyoung;Kim, Chang-Yeoul;Shim, Kwang-Bo
    • Journal of the Korean Ceramic Society
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    • v.39 no.6
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    • pp.604-609
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    • 2002
  • Nanosized $BaCeO_3$ powders with the stoichiometric composition of a molecular level were synthesized by the citrate process based on the Pechini method. Polymeric precursor was formed by use of citric acid and ethylen glycol, as chelating agent of metal ions and reaction medium, respectively. Single phase orthorhombic structured $BaCeO_3$powders, about 100 nm sized and uniform shaped were obtained through the calcination of the polymeric precursor at $900^{\circ}C$ for 4 h. Extremely small quantities of carbonate ions($CO_^{2-}$) were completely decomposed at over $1100^{\circ}C$. The mean size of the powders was increased twice, however, it has very uniform distribution in its size and shape.

Electrical Properties and Structures of Spinel Type LiMn$_{2-y}$M$_y$O$_4$(M=Cr$^{3+}$) Doped with Transition Metal (전이금속으로 치환된 Spinel형 LiMn$_{2-y}$M$_y$O$_4$(M=Cr$^{3+}$)의 구조 및 전기적 성질)

  • 형경우;김중헌;권태윤
    • Journal of the Korean Ceramic Society
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    • v.36 no.9
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    • pp.930-936
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    • 1999
  • For LiMn2O4 based spinel structures the stoichiometric reaction conditions need be considered carefully because the electrical properties depend on the structural stability. In order to obtain the homogeneous compound the Pechini process was chosen which could obtain a stoichiometry phase even low temperature and dependency of the synthetic condition on structural stability and electrochemical performance was investigated. X-ray diffraction studies showed that the compounds doped with transition metal have smaller lattice constants than those un doped. The dc conductivity was evaluated by a four probe method in the low and high temperature region respectively. The variations of basal spacings for the cathode were detected to be dependent on the extent of current flows (under dc)

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AC & DC Electrical Characterization of PTC $BaTiO_3$ and Electrodes (PTC $BaTiO_3$ 및 전극의 직류 및 교류 특성)

  • 전표용;최경만
    • Journal of the Korean Ceramic Society
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    • v.28 no.2
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    • pp.101-108
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    • 1991
  • 0.2 mo1% La doped BaTiO3 samples were prepared by a wet chemical process (Pechini process) and electrical conductivity were measured from annealing temperatures(800-110$0^{\circ}C$) to room temperature continuously. 2 probe I-V characteristics showed that Pt electrodes were non-ohmic below about 80$0^{\circ}C$ for Ladoped sample. I-V curves showed varistor behavior and breakdown voltages showed PTC-like behavior. AC complex impedance of 0.2 La and 0.05 Mn mo1% doped BaTiO3 samples with three different electrodes (electroless Ni, Pt, Ag electrodes) were measured with temperature variation. Complex impedance plots showed that the samples with electroless Ni electrodes have negligible electrode resistance. Samples with Ag or Pt paste electrodes showed large electrode resistance. PTC effect, which is defined as the ratio of maximum resistance to minimum resistance, was found to be less than 10 for 0.2 mo1% La doped dense sample however greater than 105 with codoping of 0.05 mo1% Mn and 0.2 mol% La.

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Synthesis characterization of a high conductivity LSCF cathode materials and electrochemical studies for IT-SOFC (중.저온 고체산화물 연료전지용 고전도성 공기극 소재 합성 및 전기화학적 특성 평가)

  • Kim, Hyoshin;Lee, Jongho;Kim, Ho-Sung;Lee, Yunsung
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.139-139
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    • 2010
  • LSM is widely used as a cathode material in SOFC, because of its high electrochemical activity, good stability and compatibility with YSZ electrolyte at high temperature. However, LSM in traditional cathode materials will not generate a satisfactory performance at intermediate temperature. In order to reduce the polarization resistance of cell with the operating temperature of SOFC system, the cathode material of LSCF is one of the most suitable electrode materials because of its high mixed ionic and electronic conductivity. In this report, cathode material, $La_{0.6}Sr_{0.4}Co_{0.2}Fe_{0.8}O_3$ powder for intermediate temperature SOFC was synthesized by Pechini method using the starting materials such as nitrate of La, Sr, Co and Fe including ethylene glycol, etc. As a result, the synthesized powder that calcined above $700^{\circ}C$ exhibits successfully perovskite structure, indicating phase-pure of LSCF. Moreover, the particle size, surface area, crystal structure and morphology of the synthesized oxide powders were characterized by SEM, XRD, and BET, etc. In order to evaluate the electrochemical performance for the synthesized powder, slury mixture using the synthesized cathode material was coated by screen-printing process on the anode-supported electrolyte which was prepared by a tape casting method and co-sintering. Finally, electrochemical studies of the SOFC unit cell, including measurements such as power density and impedance, were performed.

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Sintering Behavior and Electrical Properties of Strontium Titanate-Based Ceramic Interconnect Materials for Solid Oxide Fuel Cells (고체산화물 연료전지용 Strontium Titanate 세라믹 접속자 소재의 소결 거동 및 전기적 특성)

  • Park, Beom-Kyeong;Lee, Jong-Won;Lee, Seung-Bok;Lim, Tak-Hyoung;Park, Seok-Joo;Song, Rak-Hyun;Shin, Dong-Ryul
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.11a
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    • pp.80.1-80.1
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    • 2010
  • A strontium titanate ($SrTiO_3$)-based material with a perovskite structure is considered to be one of the promising alternatives to $LaCrO_3$-based materials since $SrTiO_3$ perovskite shows a high chemical stability under both oxidizing and reducing atmospheres at high temperatures. $SrTiO_3$ materials exhibit an n-type semiconducting behavior when it is donor-doped and/or exposed to a reducing atmosphere. In this work, $Sr_{1-x}La_xTi_{1-y}M_yO_3$ materials doped with $La^{3+}$ in A-sites and aliovalent transition metal ions ($M^{n+}$) in B-sites were synthesized by the modified Pechini method. The X-ray diffraction analysis indicated that the materials synthesized by the Pechini process exhibited a single curbic perovskite-type structure without any impurity phases, and are tolerant, to some extent, to cation doping. The sintering behaviors of $Sr_{1-x}La_xTi_{1-y}M_yO_3$ in $H_2/N_2$ and air were characterized by dilatometry and microstructural observations. The electrical conduction mechanism and the dopant effect are discussed based on the defect structures and the electrical conductivities measured at various oxygen partial pressures and temperatures.

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Characterization of Chemically Stabilized $\beta$-cristobalite Synthesized by Solution-Polymerization Route

  • Lee, Sang-Jin
    • The Korean Journal of Ceramics
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    • v.3 no.2
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    • pp.116-123
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    • 1997
  • A chemically stabilized $\beta$-cristobalite, which is stabilized by stuffing cations of $Ca^{2+}$ and $Al^{3+}$, was prepared by a solution-polymerization route employing Pechini resin or PVA solution as a polymeric carrier. The polymeric carrier affected the crystallization temperature, morphology of calicined powder, and particle size distribution. In case of the polyvinyl alcohol (PVA) solution process, a fine $\beta$-cristobalite powder with a narrow particle size distribution (average particle size : 0.3$\mu\textrm{m}$) and a BET specific surface area of 72 $\m^2$/g was prepared by an attrition-milling for 1 h after calcination at 110$0^{\circ}C$ for 1h. Wider particle size distribution and higher specific surface area were observed for the $\beta$-cristobalite powder derived from Pechini resin. The cubie(P1-to-tetraganalb) phase transformation in polynystalline $\beta$-cristobalite was induced at approximately 18$0^{\circ}C$. Like other materials showing transformation toughening, a critical size effect controlled the $\beta$-to-$\alpha$ transformation. Densifed cristobalite sample had some cracks in its internal texture after annealing. The cracks, occurred spontaneoulsy on cooling, were observed in the sample with an average grain sizes of 4.0 $\mu\textrm{m}$ or above. In case of the sintered cristobalite having a composition of CaO.$2Al_2O_3$.40SiO$_2$, small amount of amorphous phase and slow grain growth during annealing were observed. Shear stress-induced transformation was also observed in ground specimen. Cristobalite having a composition of CaO.2Al2O3.80SiO2 showed a more sensitive response to shear stress than the CaO.$2Al_2O_3$.40SiO$_2$ type cristobalite. Shear-induced transformation resulted in an increase of volume about 13% in $\alpha$-cristobalite phase on annealing for above 10 h in the case of the former composition.

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A Study on the Synthesis of Gd-doped $CeO_2$ and Sr-doped $LaMnO_3$ Powders and Phase Stability in Their Interface (Gd-doped $CeO_2$ 와 Sr-doped $LaMnO_3$ 분말의 합성 및 그 계면에서의 상 안정성 연구)

  • 정승훈;김남진;이덕열
    • Journal of the Korean Ceramic Society
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    • v.34 no.6
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    • pp.652-658
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    • 1997
  • The phase stability in the interface of Sr-doped LaMnO3(LSM)/Gd-doped CeO2(CGO) was examined in this study in order to check the feasibility of using LSM as the cathode material in a low-temperature SOFC(solid oxide fuel cell) using CGO as the electrolyte. For the purpose, CGO powders of Ce0.82Gd0.18O0.91 and two LSM powders having different compositions, La0.9Sr0.1MnO3(LSM10) and La0.5Sr0.5MnO3(LSM50), were synthesized using Pechini method. Then, specimens having the LSM/CGO interface were prepared, heat-treated at 130$0^{\circ}C$ for up to 3 days, and analyzed by XRD and STEM/EDX. Face-centered cubic CGO powders of less than 10 nm size were obtained by calcination of polymeric precursor formed in the process at 45$0^{\circ}C$. Higher calcination temperature of $700^{\circ}C$ was necessary for monoclinic LSM10 and cubic LSM50 powders. LSM powders were coarser than CGO and observed to be in the range of 50~100 nm. No trace of LSM-CGO interaction product was found in the XRD pattern. Also it was known from the concentration profile in the vicinity of the interface that interdiffusion was occurred over only a small penetration depth of ~100 nm order.

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Fabrication of Al2O3/ZrO2Ceramics by the Polymerization Dispersion Process (ZrO2의 고분자화 분산법을 이용한 Al2O3/ZrO2요업체의 제조)

  • Cho, Myung-Je;Hwang, Kyu-Hong;Lee, Jong-Kook
    • Journal of the Korean Ceramic Society
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    • v.41 no.4
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    • pp.284-288
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    • 2004
  • To improve mechanical properties of $Al_2$O$_3$/ZrO$_2$composites have been controlled dispersion of ultra low size ZrO$_2$ particles in $Al_2$O$_3$ ceramics by polymeric precursor method (Pechini process). In case of coprecipitation or mechanical mixing of ZrO$_2$ powders with $Al_2$O$_3$, homogeneous dispersion and controlling the ZrO$_2$ size were relatively difficult due to high sintering temperature. So the polyesterization process of Zr/Y(NO$_3$)$_3$-citric acid solution in ethylene glycol with the commercial sub-micron sized o(-alumina powder (Sumitomo AES-11(0.4 ${\mu}{\textrm}{m}$)) was adopted in order to obtain homogeneous dispersion of ZrO$_2$ in A1203. By this partial polyesterization process, the homogeneous dispersion of relatively low sized ZrO$_2$in $Al_2$O$_3$/ZrO$_2$composites was achieved at 1450∼1$600^{\circ}C$ of sintering temperature range and their mechanical properties were measured.

Thermal Decomposition and Sintering Characteristics of Cr-Deficient $(La,Ca)CrO_3$ (크롬부족 (란탄, 칼슘)크로마이트의 열분해과정 및 소결특성)

  • 이상기;조성걸
    • Journal of the Korean Ceramic Society
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    • v.34 no.11
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    • pp.1182-1186
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    • 1997
  • La0.8Ca0.2Cr0.98O3 powder was prepared using the modified Pechini process. Various crystalline phases formed during thermal decomposition were investigated. (La,Ca)CrO4 phase, first formed from the precursor, was transformed to (La,Ca)CrO3 and CaCrO4 above 80$0^{\circ}C$, which remained up to 110$0^{\circ}C$. However, only (La,Ca)CrO3 phase consisting of orthorhombic and intermediate rhombohedral polymorphs was observed after sintering at 125$0^{\circ}C$. The specimens sintered at 140$0^{\circ}C$ exhibited 98% of relative density and rather wide grain size distribution with average grain size of 3-4 ${\mu}{\textrm}{m}$. Densification and grain growth of the specimens observed above 125$0^{\circ}C$ were presumably attributed to liquid phase sintering resulted from melting of Ca3(CrO4)2 phase.

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