• 한국세라믹학회지
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• 제47권2호
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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%.

• 한국세라믹학회지
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• 제32권4호
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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.

• 한국재료학회:학술대회논문집
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• 한국재료학회 2010년도 춘계학술발표대회
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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.

• 한국전기전자재료학회논문지
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• 제15권1호
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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$0^{\circ}C$

• 한국세라믹학회지
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• 제33권7호
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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$^{\circ}C$)

• 한국세라믹학회지
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• 제30권6호
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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.

• The Korean Journal of Ceramics
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• 제4권3호
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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.

• 분석과학
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• 제10권1호
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• pp.31-34
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• 1997

pH 4~5에서$ Ti^{4+}$ 이온을 여분의 옥살산 음이온으로 안정화시킨 다음 같은 당량의 $Ba^{2+}$ 이온이 첨가된 환경수 시료와 일시에 혼합시켜 줌으로써 barium titanate의 선구물질인 barium titanyl oxalate를 합성하였다. 이 때 환경수 시료 속에 미량으로 존재하는 $Cd^{2+}$ 및 $Pb^{2+}$ 이온이 정량적으로 공침되었으며, 이 공침법은 이들 원소의 분석을 위한 사전 농축법으로 활용 가능하였다.

• 한국세라믹학회지
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• 제26권3호
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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.

• 분석과학
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• 제10권3호
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• pp.203-208
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• 1997

출발물질로 $BaCl_2$와 $TiCl_4$를 사용하고 침전제로 dimethyl oxalate(DMO)를 사용하여 균일침전법에 의해 barium titanyl oxalate(BTO)를 제조하였다. 반응조건을 변화시켜 가면서 실험을 수행한 결과 반응 온도가 높을수록, [DMO]/[$Ba^{2+}+Ti^{4+}$]의 비율이 증가할수록 핵 형성시간이 단축되었으며 BTO 입자가 unimodal에서 bimodal을 거쳐 넓은 범위의 unimodal로 전환하는 속도가 빨랐다. 균일침전법으로 얻은 BTO를 $900^{\circ}C$에서 하소하여 얻은 barium titanate(BT)의 입자 크기는 통상의 공침법으로 합성한 BT 입자보다 큰 형태를 나타냈으며, 결정상은 tetragonal이었다. 또한 교반이 BTO 및 BT 분말의 특성에 큰 영향을 줌을 발견하였다.