• Title/Summary/Keyword: Oxalate method

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Synthesis of High Tc Superconductor YBa2Cu3O7-$\delta$ by Oxalate Coprecipitation Method I. Theoretical Considerations based on Analytical Chemistry (옥살레이트 공침전법에 의한 고온 초전도체 YBa2Cu3O7-$\delta$의 합성 I. 분석화학적 측면의 이론적 고찰)

  • 김배환;김배연;김창은;최진호
    • Journal of the Korean Ceramic Society
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    • v.26 no.1
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    • pp.91-99
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    • 1989
  • The concentrations of hydroxide, carbonate and oxalate for Y(III), Ba(II) and Cu(II) ions in an aqueous solution have been theoretically calcuated with respect to pH and their solubility diagram could be obtained. The optimum pH ofr oxalate coprecipitates at room temperature was estimated as<4, which was not influenced by carbonates and hydroxides in H2O solvent. The yield is dependent on the concentration of added oxalic acid, but the concentration of oxalic acid was fixed as 0.1M in this calculation for simplicity.

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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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A Study on the Dielectric Properties of $SrTiO_3$ Sintered Body Synthesized by Oxalate Method (수산염법으로 합성한 $SrTiO_3$ 소결체의 유전특성에 관한 연구)

  • 김병호;이만규;김석우
    • Journal of the Korean Ceramic Society
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    • v.28 no.3
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    • pp.215-224
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    • 1991
  • The synthesis of SrTiO3 powders having high purity and homogeneous submicron particle size was attempted by the oxalate method. The microstructure and dielectric properties of SrTiO3 based boundary layer capacitor (BLC) were investigated. Strontium titanyl oxalate[SrTiO(C2O4)2.4H2O] was prepared from the mixing solution of (Sr, Ti) using oxalic acid(H2C2O4) as a precipitating agent at 8$0^{\circ}C$. The crystalline SrTiO3 powder was obtained by thermal decomposition of the precipitate above $600^{\circ}C$. The crystalline SrTiO3 powder containing Nb2O5 as a dopant, TiO2 and SiO2 as additives was sintered at 1360~144$0^{\circ}C$ in the reducing atmosphere to get semiconductive SrTiO3. Insulating material containing PbO-Bi2O3-B2O3 frit was printed on the sintered semiconductive SrTiO3 and fired at 120$0^{\circ}C$ for 2h to get the grain boundary diffusion.

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Development of the Dissolution Tests for Nafronyl Oxalate Capsules and Tramadol Hydrochloride Capsules (수산나프로닐 캡슐 및 염산트라마돌 캡슐의 용출시험에 관한 연구)

  • Hwang, Joung-Boon;Moon, Hyun-Ju;Go, Seo-Youn;Jang, Gi-Uk;Lee, Kyu-Ha;Sohn, Kyung-Hee;Kim, In-Kyu;Cho, Dae-Hyun
    • YAKHAK HOEJI
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    • v.55 no.5
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    • pp.411-418
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    • 2011
  • The dissolution test method and an analytical procedure by HPLC were developed and validated for nafronyl oxalate capsules and tramadol hydrochloride capsules. These drugs were not yet characterized by the dissolution specifications in the Korean Pharmaceutical Codex. So, with each reference and test drugs, we did the preliminary and standard experiments based on the Korean Pharmacopeia Guideline of dissolution testing for solid oral dosage forms. The dissolution test for nafronyl oxalate capsules was carried out under sink conditions as follows: dissolution medium phosphate buffer pH 6.8, paddle rotation speed 100 rpm and vessel volume 900 ml. More than 80% of its label amount was released within 30 min in this method. Also the dissolution test for tramadol hydrochloride capsules was carried out under sink conditions as follows: dissolution medium water, paddle rotation speed 50 rpm and vessel volume 900 ml. More than 90% of its label amount was released within 15 min in this method. The dissolution samples were analyzed with a validated HPLC analytical procedure. The analytical methodology showed acceptable values in terms of specificity, linearity, precision and accuracy. The dissolution test methods described above were adequate for the purpose and may be proposed as a pharmacopeial standard to assess the performance of nafronyl oxalate capsules and tramadol hydrochloride capsules. Furthermore, the outcomes of this study were expected to help create an environment where safe and high quality drugs would be distributed on the domestic market making contributions to advancing public health.

A Study on the Agglomeration of BaTiO3 Nanoparticles with Differential Synthesis Route (나노입자 합성방법에 따른 타이타늄산바륨 나노입자뭉침 현상 연구)

  • Han, W.-J.;Yoo, B.-Y.;Park, H.-H.
    • Journal of the Microelectronics and Packaging Society
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    • v.22 no.2
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    • pp.33-39
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    • 2015
  • $BaTiO_3$ is typical ferromagnetic materials with dielectric constant of above 200. $BaTiO_3$ nanoparticles applications are available for multiple purposes such as nanocapacitors, ferroelectric random access memories, and so on. Applications are is diverse from the dispersion of nanoparticles depending on the route of synthesis. In this study, $BaTiO_3$ nanoparticles were synthesized by two different methods such as oxalate method and sol-gel process (ambient condition sol method). Particle size and dispersion condition were studied according to the preparation method and capping agent. Poly vinyl pyrrolidone (PVP) was used as a capping agent in oxalate method and tetrabutylammonium hydroxide (TBAH) used as a capping agent in sol-gel process each. Cubic crystal structure of $BaTiO_3$ phase could be confirmed by X-ray diffraction analysis. Fourier transform-infrared spectroscopy was employed for the confirmation of the capping agent and $BaTiO_3$ nanoparticles. The particle size and distribution analysis was also performed by particles size analyzer and scanning electron microscope.

The Powder Synthesis of (Bi,Pb)-2223 System Superconductor by Oxalate Method and Thick Film Preparation (옥살산염법에 의한 (Bi, Pb)-2223계 초전도 분말 합성과 후막 제조)

  • 하성원;김형태;이응상
    • Journal of the Korean Ceramic Society
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    • v.34 no.10
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    • pp.1083-1091
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    • 1997
  • As one of the chemical powder fabrication methods, the powder preparation method by using oxalate has the following advantages; (1) easy to control the chemical stoichiometry, (2) easy to fabricate homogeneous and fine particles, and (3) easy to be thermaly decomposed at low temperature. In the present study, the initial morphology and size distribution of the powder were controlled and the homogeniaty was improved. By carefully controlling the pH with NH4OH, the Bi(Pb)-Sr-Ca-Cu-O superconducting powders were prepared and investigated for their properties. The microstructures and the superconducting properties of the pelletized samples were investigated. Also, the microstructures and electrical properties of the samples prepared by tape casting method were investigated. The fabricated powders were spherical with less than 400 nm, but most of them were agglomerated to be 1~3 ${\mu}{\textrm}{m}$ in size. The critical temperature of the pelletized sample annealed at 84$0^{\circ}C$ for 72 hours in air was 110K. And the critical currents of annealed samples in air prepared by tape casting process for 24 hours and 72 hours were 0.6 A (Jc=600A/$\textrm{cm}^2$) and 1.9A (Jc=1, 900A/$\textrm{cm}^2$) respectively.

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Effect of Reaction Conditions on the Particle Properties for Synthesis of Stabilized Zirconia by Modified Oxalate Method

  • Park, Hyun-wook;Lee, Young Jin;Kim, Jin-Ho;Jeon, Dae-Woo;Hwang, Hae Jin;Lee, Mi Jai
    • Journal of the Korean Ceramic Society
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    • v.53 no.5
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    • pp.529-534
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    • 2016
  • Nanocrystalline powder of zirconia stabilized with 8 mol% yttria (YSZ) has been synthesized through oxalate process using $ZrOCl_2{\cdot}8H_2O$ and $Y(NO_3)_3{\cdot}6H_2O$ as starting materials. Understanding of the characteristic changes of YSZ powder as a function of processing conditions is crucial in developing dense and porous microstructures required for fuel cell applications. In this research, microstructure change, surface area, particle shape and particle size were measured as a function of different processing conditions such as calcination temperature, stirring speed and concentration of starting materials. The resultant crystallite sizes were calculated by XRD-LB (X-Ray Diffraction Line-Broadening) method, BET method, and morphology of the crystal was observed in TEM and FE-SEM. The TEM examination showed that the powder synthesized with 0.7 M of YSZ concentration had a spherical morphology with sizes ranging from 20 to 40 nm. However, the powder was gradually aggregated above 1.0 M of YSZ concentration with the aggregation being intensified as the YSZ concentration was increased.

Effect of $ZrO_2$ Addition on the Synthesis and Microwave Dielectric Properties of $Ba_2Ti_9O_{20}$ Fabricated by Oxalate method (수산염법에 의한 $Ba_2Ti_9O_{20}$의 합성과 유전특성에 미치는 $ZrO_2$ 첨가의 영향)

  • 박재원;이헌식;이병하
    • Journal of the Korean Ceramic Society
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    • v.31 no.8
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    • pp.835-840
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    • 1994
  • In this study, the synthesis of Ba2Ti9O20 powder having chemically homogeneous and highly pure fine particle size distribution was attempted by the oxalate method. And the effects of ZrO2 addition was investigated. The four compositions (X=0, 0.028, 0.048, 0.068) of Ba2(Ti9-x, Zrx)O20 were prepared by precipitation reaction of BaCl2, TiCl4, and ZrOCl2, with oxalic acid and NH4OH acting as a precipitating agent and a pH regulator respectively, in aqueous solution. In case of 4.8 mol% ZrO2 addition, the single phase Ba2Ti9O20 was obtained at 120$0^{\circ}C$ and its dielectric properties was excellent showing K=40.5, Q=4621 at 5.4 GHz.

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Synthesis and Characterization of KTiNbO5 Nano-particles by Novel Polymerizable Complex Method

  • Wang, Ning-Ning;Lan, Yun-Xiang;He, Jie;Dong, Rui;Hu, Jin-Song
    • Bulletin of the Korean Chemical Society
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    • v.34 no.9
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    • pp.2737-2740
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    • 2013
  • The layered $KTiNbO_5$ was successfully synthesized with titanium(IV) isopropoxide and niobium oxalate by a novel polymerized complex (PC) method. The morphology and structure of the as-prepared sample was characterized by means of High-Resolution Transmission Electron Microscope, powder X-ray diffraction, and Laser Raman Spectroscopy. The spectral response characteristic was recorded by using UV-vis Diffuse Reflectance Spectroscopy. Results show that $KTiNbO_5$ as-prepared by PC method presents an uniform morphology of nano-particles, the mean particle sizes is ca. 28 nm corresponding to the (002), and the crystal structure can be well indexed to the orthorhombic phase. The sample as-prepared by PC method has higher band gap energy than that of the sample prepared by a solid-state reaction method due to the quantum size effect.