• Title/Summary/Keyword: Oxalate coprecipitation

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Preparation and Characterization of Europium-doped Gadolinium Oxide Phosphors Using Oxalate Coprecipitation Method

  • Park, In-Yong;Lee, Jong-Won
    • Journal of the Korean Ceramic Society
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    • v.47 no.2
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    • pp.177-182
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    • 2010
  • To synthesize $Gd_2O_3:Eu^{3+}$ phosphor, gadolinium-europium oxalate precursors were prepared from oxalic acid, NaOH or aqueous ammonia via coprecipitation method. The obtained precursors were heat-treated and then characterized by XRD, SEM and PL. The kinds and amounts of coprecipitant (NaOH or aqueous ammonia) were found to affect the powder morphology and properties of gadolinium-europium oxalate precursors. Two crystalline precursors and one amorphous precursor were synthesized. The nanometer-sized amorphous gadolinium-europium oxalate precursor was first prepared using the oxalate coprecipitation technique. The calcined powders obtained from the amorphous precursor were nearly spherical in shape, and a narrow size distribution was obtained. The NaOH coprecipitant was more effective in the preparation of nanometer-sized spherical powders. A thermal decomposition process was conducted for the three kinds of precursors. The photoluminescence property was also measured as a function of europium content, and concentration quenching occurred for samples with europium concentrations of over 10 mol%.

Synthesis of $\beta$-Alumina By Oxalate Coprecipitation Method and Its Crystallization Behavior (Oxalate 공침법에 의한 $\beta$-Alumina 합성과 결정화 거동)

  • 박용민;양유철;김형욱;박성수;손영국
    • Journal of the Korean Ceramic Society
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    • v.32 no.4
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    • pp.455-461
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    • 1995
  • To investigate the synthesis of $\beta$-Al2O3 and its crystallization behavior by oxalate coprecipitation method, the optimum pH range for oxalate coprecipitates has been theoretically calculated from the solubility products and the equilibrium constans of each metal ionic species and their solubility diagram wa obtained. The optimum pH range for oxalate coprecipitates at room temperature was estimated as <4. In experiment, we found that the optimum condition for oxalate coprecipitates was pH<1, which was not doped with pH controller. The Na+ ions were easily exchanged for the NH4+ ions of NH4OH which was used as pH controller, and those NH4+ ions were supposed to affect the crystallization behavior of $\beta$-Al2O3. The thermal decomposition of all complexes was almost complete below 40$0^{\circ}C$. The primary product of the decomposition process was m-Al2O3, which transformed to $\beta$"- or $\beta$-Al2O3 at temperature higher than 100$0^{\circ}C$. We found that the powder prepared at 120$0^{\circ}C$ had only $\beta$"- and $\beta$-Al2O3.EX>-Al2O3.

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Synthesis of Multi-component Olivine by a Novel Mixed Transition Metal Oxalate Coprecipitation Method and Electrochemical Characterization

  • Park, Yeong-Uk;Kim, Jong-Sun;Gwon, Hyeok-Jo;Seo, Dong-Hwa;Kim, Seong-Uk;Hong, Ji-Hyeon;Gang, Gi-Seok
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2010.05a
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    • pp.37.1-37.1
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    • 2010
  • The multi-component olivine cathode material, $LiMn_{1/3}Fe_{1/3}Co_{1/3}PO_4$, was prepared via a novel coprecipitation method of the mixed transition metal oxalate, $Mn_{1/3}Fe_{1/3}Co_{1/3}(C_2O_4){\cdot}2H_2O$. The stoichiometric ratio and distribution of transition metals in the oxalate, therefore, in the olivine product, was affected sensitively by the environments in the coprecipitation process, while they are the important factors in determining the electrochemical property of electrode materials with multiple transition metals. The effect of the pH, atmosphere, temperature, and aging time was investigated thoroughly with respect to the atomic ratio of transition metals, phase purity, and morphology of the mixed transition metal oxalate. The electrochemical activity of each transition metal in the olivine synthesized through this method clearly was enhanced as indicated in the cyclic voltammetry (CV) and galvanostatic charge/discharge measurement. Three distinctive contributions from Mn, Fe, and Co redox couples were detected reversibly in multiple charge and discharge processes. The first discharge capacity at the C/5 rate was $140.5\;mAh\;g^{-1}$ with good cycle retention. The rate capability test showed that the high capacity still is retained even at the 4C and 6C rates with 102 and $81\;mAh\;g^{-1}$, respectively.

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Fine Powder Synthesis and It`s Sintering Characteristics of Gd2O3Doped CeO2 by the Oxalate Coprecipitation Method (Oxalate 공침법에 의한 Gd2O3Doped CeO2의 미분말 합성 및 그 소결특성)

  • 최광훈;박성용;이주진
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.15 no.1
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    • pp.46-55
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    • 2002
  • 10mo1% Gd$_2$O$_3$ doped CeO$_2$ fine powders were synthesized by the oxalate coprecipitation method. The characteristics and sintering behavior of fine powders were investigated. The oxalate precipitates had the specific surface area of 150$m^2$/g, and appeared to be fine and spherical primary particles with a size of approximately 5.5nm. The decomposition of the precipitates occurred from a temperature around 30$0^{\circ}C$ and it was completed below 40$0^{\circ}C$, resulted in the formation of the oxide. The calcination temperature of the fine powders was suitable at 77$0^{\circ}C$. By introducing fine powders washed with alcohol and ball-milling process after calcination, the sintered body was possible to attain the value of 97% of the theoretical density at low temperature of 130$0^{\circ}C$

A Study on the Synthesis and Properties of (Ba,Pb)$TiO_3$Powder by Modified Oxalate Process (Modified Oxalate Process에 의한 (Ba,Pb)$TiO_3$ 분말합성 및 특성에 관한 연구)

  • ;;;Y, Torii
    • Journal of the Korean Ceramic Society
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    • v.33 no.7
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    • pp.743-754
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    • 1996
  • In this study (Ba1-xPbx)TiO3 was synthesized by modified oxalate process in order to prevent vaporization of PbO through low temperature synthesis climinate Cl ion reproducibly substitute Pb for by and uniformly distribute ion (Ba1-xPbx)TiO3 was synthesized by coprecipitation of lead acetate barium acetate and ammonium titanyl oxalate have been used as starting materials. The substitution of Pb for Ba was reproducibly possible synthetic temperature of perovskite structure becomes lowed as the Pb concentration increases and fine partic-les (specific surface are :7.2 cm2/g) were obtained, BaTiO3 powders calcined at 90$0^{\circ}C$ for 3 hours were cubic from in XRD analysis and as Pb content was increases evident split of tetragonal peaks could be observed The optimum conditions to synthesize (Ba,Pb)TiO3 powder are the followings ; synthesis temperature (5$^{\circ}C$)

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MnZn Ferrite Preparation by Coprecipitation Method (공침법에 의한 MnZn Ferrite 분말제조 연구)

  • 엄태형;고성만;서동수;양준환;박균하
    • Journal of the Korean Ceramic Society
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    • v.30 no.6
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    • pp.478-484
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    • 1993
  • The influence of reaction conditions on the MnZn ferrite coprecipitation process were investigated using mixed metla sulfate solution and ammonium oxalate. In order to minimize the metallic ion losses and to control the particle size, the optimum reaction conditions were as follows; reaction temperature $25^{\circ}C$, metal sulfate concentration 0.3M, molar ratio of ammonium oxalate/mixed metal sulfate 1.1:1. The production yield was as high as 97.6% of theoretical yield at optimum reaction condition.

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Preparation of Proton-Conducting Gd-Doped Barium Cerate by Oxalate Coprecipitation Method

  • Yong Sung Choi;Soo Man Sim
    • The Korean Journal of Ceramics
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    • v.4 no.3
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    • pp.213-221
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    • 1998
  • $BaCe_{0.9}Gd_{0.1_O_{2.95}$ powder was synthesized by oxalate coprecipitation method. Precipitate with a stoichimetric ratio of the cations was prepared by adding a mixture of Ba, Ce and Gd nitrate solution to an oxalic acid solution at pH 4. Reaction between the constituent oxides to form a perovskite phase was initiated at $800^{\circ}C$ and a single phase $BaCe_{0.9}Gd_{0.1_O_{2.95}$ powder having good sinterability was obtained after calcination at $1000^{\circ}C$. Sintering green compacts of this powder for 6 h showed a considerable densification to start at $1100^{\circ}C$ and resulted in 93% and 97% relative densities at $1300^{\circ}$ and at $1450^{\circ}C$, respectively. Whereas the power compacts prepared by solid state reaction had lower relative densities, 78% at $1300^{\circ}$and 90% at $1450^{\circ}C$. Fine particles of $CeO_2$ second phase were observed in the surface of the sintered compacts. This was attributed to the evaporation of BaO from the surface that had been exposed during thermal etching.

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Separation of $Cd^{2+}$ and $Pb^{2+}$ by means of their coprecipitation on $BaTiO(C_2O_4)_2{\cdot}4H_2O$ precipitate ($BaTiO(C_2O_4)_2{\cdot}4H_2O$ 공침법에 의한 $Cd^{2+}$$Pb^{2+}$의 분리)

  • Min, Chonkyu;Noh, Taeyong;Lee, Chul
    • Analytical Science and Technology
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    • v.10 no.1
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    • pp.31-34
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    • 1997
  • Barium titanyl oxalate which is a precursor of barium titanate has been precipitated at pH 4~5 by a rapid addition of aqueous titanyl oxalate solution to artificial environmental water samples containing equivalent weight of $Ba^{2+}$ ions. Quantitative recoveries of $Cd^{2+}$ and $Pb^{2+}$ from the water samples has been confirmed and found to be usable as a possible method of preconcentration for their determination.

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Synthesis of High Tc Superconductor YBa2Cu3O7-$\delta$ by Oxalate Coprecipitation Method II. The Effect of Cu2+-Oxalate-Complex Formation for the Solubilities of Y3+ and Ba2+ (Oxalate공침법에 의한 고온 초전도체 YBa2Cu3O7-$\delta$의 합성 II. Cu2+-Oxalate-Complex가 Y3+ 및 Ba2+의 용해도에 미치는 영향)

  • 최진호;김배환;최규원
    • Journal of the Korean Ceramic Society
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    • v.26 no.3
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    • pp.395-401
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    • 1989
  • The concentrations of Cu(II), Y(III) and Ba(II) ionic species in aqueous solution due to the formation of Cu2+-oxalate-complex have been theoretically calculated with respect to pH and their solubility diagrams could be obtained. It was verified from the calculation that the excess of Cu2+ and Ba2+ should be added in order to obtain oxalate coprecipitates with the molar ratio of Y : Ba : Cu=1 : 2 : 3. The exact amount of excess species has been calculated with respect to the initial concentrations of metal ions and pH.

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Morphology of Barium Titanyl Oxalate Produced by Homogeneous Precipitation from Acidic Solution of Dimethyl Oxalate (Dimethyl Oxalate에 의한 균일 침전법으로 생성된 Barium Titanyl Oxalate의 형태학적 연구)

  • Min, Chonkyu;Lee, Chul
    • Analytical Science and Technology
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    • v.10 no.3
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    • pp.203-208
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    • 1997
  • Barium titanyl oxalate(BTO) was precipatated by utilizing the thermal decomposition of dimethyl oxalate in acidic aqueous solution having $BaCl_2$ and $TiCl_4$. Particle morphology of BTO was influeneced by the various experimental factors. i.e.. the faster rate to nucleation with higher temperature and the higher ratio of [DMO]/[$Ba^{2+}+Ti^{4+}$] was found to correspond to the faster rate of transformation of particle size distribution from unimodal to broad unimodal through bimodal. The BT powder obtained by calcination at $900^{\circ}C$ in air consists of larger particles than BT generated by general coprecipitation method and shows tetragonal symmetry. The stirring during reaction was also found to have much effect upon characteristics of BTO and BT.

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