• Title/Summary/Keyword: coprecipitation

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Crystal Structure of $TiO_2-SnO_2$ Fine Powders Prepared by Coprecipitation (공침법에 의해 제조된 $TiO_2-SnO_2$ 미분말의 결정구조)

  • 이종흔;박순자
    • Journal of the Korean Ceramic Society
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    • v.30 no.9
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    • pp.740-746
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    • 1993
  • TiO2-SnO2 fine powders prepared by coprecipitation from TiCl4-SnCl4 aqueous solution, and their crystal structures were studied. All the TiO2-SnO2 fine powders calcined at 180~$700^{\circ}C$ showed the complete solid solution between TiO2(rutile structure) and SnO2(rutile structure). This crystal structure of TiO2-SnO2 powders is thought to be originated mainly from the heterogeneous nucleation of Ti-hydroxde on the Sn-hydroxide with coherent structure.

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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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Influence of pH on Sensitivity of $WO_3$ NO gas sensor fabricated by Sol-Coprecipitation method (Sol-Coprecipitation 법에 의한 NO 감지용 $WO_3$ 센서 제조시 pH의 영향)

  • Kim, Suk-Bong;Lee, Dae-Sik;Lee, Duk-Dong;Huh, Jeung-Soo
    • Journal of Sensor Science and Technology
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    • v.10 no.2
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    • pp.118-124
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    • 2001
  • When particles are dissolved in solution, they have different zeta-potentials depending on pH. Zeta-potential has an influence on particle separation, which can control particle size. And the size of $WO_3$ particle affects the sensitivity of $WO_3$ sensor for detecting NO gas. Therefore we study influence of pH on NO-sensing $WO_3$ gas sensor fabricated by Sol-Coprecipitation method. As pH increases from 2 to 7, dynamic mobility of $WO_3$ precursor was increased. When pH was 7, it showed the largest distribution separation. It means when pH is 7, we can make $WO_3$ powder which has smaller particle size. And it is confirmed by particle size analysis of $WO_3$ powder, X-ray diffration result of $WO_3$ sensing layer and surface morphology. It also affect NO sensing characteristics of $WO_3$ gas sensor. The sensing film synthesized at pH 7 showed the largest sensitivity.

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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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Effect of nucleating agents and stabilisers on the synthesis of Iron-Oxide Nanoparticles-XRD analysis

  • Butt, Faaz A.;Jafri, Syed M. Mohsin
    • Advances in nano research
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    • v.3 no.3
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    • pp.169-176
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    • 2015
  • Iron nanoparticles were made by using the modified coprecipitation technique. Usually the characteristics of synthesised particles depend upon the process parameters such as the ratio of the iron ions, the pH of the solution, the molar concentration of base used, type of reactants and temperature. A modified coprecipitation method was adopted in this study. A magnetic stirrer was used for mixing and the morphology and nature of particles were observed after synthesis. Nanoparticles were characterised through XRD. Obtained nanoparticles showed the formation of magnetite and maghemite under citric acid and oxalic acid as stabilisers respectively. The size of nanoparticle was greatly affected by the use of different types of stabilisers. Results show that citric acid greatly reduced the obtained particle size. Particle size as small as 13 nm was obtained in this study. The effects of different kinds of nucleating agents were also observed and two different types of nucleating agents were used i.e. potassium hydroxide (KOH) and copper chloride ($CuCl_2$). Results show that the use of nucleating agent in general pushes the growth phase of nanoparticles towards the end of coprecipitation reaction. The particles obtained after addition of nucleating agent were greater in size than particles obtained by not utilising any nucleating agent. These particles have found widespread use in medical sciences, energy conservation and electronic sensing technology.

Synthesis of Alumina-Grafted Manganese Oxide Particles Using Surfactants through Coprecipitation Method and Their Thermal Properties

  • Kwon, Boseong;Park, Jun-Hwan;Jang, Seong-Cheol;Oh, Seong-Geun
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3559-3564
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    • 2013
  • Alumina particles were grafted onto the surface of manganese oxide particles via the coprecipitation process using surfactant and cosurfactant. The phase of Mn/Al salts (Phase I) and the phase of precipitation agent (Phase II) were prepared in aqueous surfactant solution, separately. Phase II was added into Phase I and the reaction was performed to form the precursors of composites through hydrogen bonding between $Mn(OH)_2$ and $Al(OH)_3$ prepared by the reaction of Mn/Al salts with the precipitation agent. The alumina-grafted manganese oxide particles were obtained as a final product after calcination. The concentrations of Al salt and surfactant were varied to investigate their effects on the formation and the crystallinity of composites. In addition, the crystal structure of products could be controlled by changing the calcination temperature. Through thermal analyses, it was found that the thermal stability of manganese oxide was improved by the introduction of alumina on its surface.

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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Powder Preparation by Hydroxide Coprecipitation and Phase Development of Pb0.97La0.02(Zr0.64Sn0.25Ti0.11)O3 Ceramics

  • Lee, Joon-Hyung;Chiang, Yet-Ming
    • The Korean Journal of Ceramics
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    • v.4 no.3
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    • pp.260-267
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    • 1998
  • A homogeneous and stoichimetric fine powder of the ferroelectric $Pb_[0.97}La_{0.02}(Zr_{0.64}Sn_{0.25}Ti_{0.11})O_3$ (PLZST) has been prepared by the hydroxide coprecipitation method. Studies on the crystallization behavior of precursor as a function of temperature by X-ray powder diffraction and transmission electron microscopy technique were consistent with the formation of the pyrochlore phase from amorphous, initially at low temperatures around 500~$550^{\circ}C$. Further heat treatment up to $750^{\circ}C$ resulted in development of the perovskite phase with no significant pyrochlore crystallite growth. At intermediate temperatures the precursor yields a fine mixture of pyrochlore and perovskite phases. When the pyrochlore phase was heat teated in air, slight weight increase was observed in the temperature range of 300~$700^{\circ}C$, which is thought to be caused from oxygen absorption. In argon atmosphere, weight increase was not observed. On the other hand, weight loss began to occur near $700^{\circ}C$, with giving off mostly CO2 gas. This implies that the pyrochlore phase seems to be crystallorgraphycally and thermodynamically metastable. An apparent activation energy of 53.9 ㎉/mol was estimated for the pyrochlore-perovskite phase transformation.

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Preparation of $Al_2O_3$-$ZrO_2$ Composite Powders by the Use of Emulsions : III. Emulsion-Coprecipitation Method (에멀젼을 이용한 $Al_2O_3$-$ZrO_2$복합분체의 제조 : III. 에멀젼-공침법)

  • 현상훈;김의수
    • Journal of the Korean Ceramic Society
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    • v.27 no.4
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    • pp.487-494
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    • 1990
  • $Al_2O_3$-20w/o $ZrO_2$ composite powders were prepared by the emulsion-coprecipitation method and the effects of preparative conditions on powder characteristics were investigated. In the preparation of $Al_2O_3$-$ZrO_2$ composite powders, toluene was used instead of kerosene as the oil phase in emulsions. After coprecipitation, the emulsion was easily broken into a single liquid phase by adding methanol, and then precipitates could be effectively collected by filteration. The fact that all $ZrO_2$ phases present at room temperature in composite powders calcined at $1100^{\circ}C$ after washed by methanol had a tetragonal structure confirmed that methanol-washing enhanced the dispersibility of fine $ZrO_2$ particles in $Al_2O_3$ matrix. $Al_2O_3$-$ZrO_2$ composite powders were spherical particles of 0.2${\mu}{\textrm}{m}$ diameter. Pellets sintered at $1650^{\circ}C$ for 2hrs showed the relative theoretical density of 97.3% and the fracture toughness of 5.01MN/$m^{3/2}$.

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Synthesis of Ag-Hydroxyapatite Antibiotic Material by Coprecipitation Method (공침법을 이용한 은-수산화아파타이트 항균소재의 제조)

  • Jang, Kwang-Kyu;Shin, Hun Yong
    • Korean Chemical Engineering Research
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    • v.45 no.5
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    • pp.473-478
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    • 2007
  • Antibiotic composite was synthesized by coprecipitation of silver nitrate into hydroxyapatite. Adsorbed amount of silver ion was examined by the variation of concentration of silver nitrate, temperature, pressure and curing time. Optimum condition for silver-hydroxyapatite adsorption could be achieved. Physical and chemical characteristic properties of synthesized silver-hydroxyapatite were tested by ICP-MS, SEM-EDAX, DSC and XRD. Antibiotic properties for gram positive staphylococcus aureus (ATCC 6538) and gram negative escherichia coli (ATCC 25922) were tested by shake flake method.