• Title/Summary/Keyword: 단일상 합성법

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Crystal Structure and Magnetic Properties of Iron Doped La-Sr-Mn-O (철을 미량 치환한 La-Sr-Mn-O의 결정학적 및 자기적 특성 연구)

  • Ahn, Geun-Young;Shim, In-Bo;Kim, Sam-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.12 no.1
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    • pp.14-19
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    • 2002
  • The iron-doped perovskite La$_{0.67}$Sr$_{0.33}$Mn$_{0.99}$$^{57}$Fe$_{0.01}$O$_3$compound has been studied by x-ray diffraction, Mossbauer spectroscopy, and vibrating sample magnetometry. The single phase of the polycrystalline La$_{0.67}$Sr$_{0.33}$Mn$_{0.99}$$^{57}$Fe$_{0.01}$O$_3$powder has been prepared by a waterbased solgel method. Crystalline La$_{0.67}$Sr$_{0.33}$Mn$_{0.99}$$^{57}$Fe$_{0.01}$O$_3$was a rombohedral structure with lattice parameters a$_{0}$=5.480 $AA$, $alpha$=60.259$^{circ}$. Mossbauer spectra of La$_{0.67}$Sr$_{0.3}$/Mn$_{0.99}$$^{57}$Fe$_{0.01}$O$_3$have been taken at various temperatures ranging from 20 to 400 K. As the temperature increases toward the Curie temperature, T$_{c}$=375 K, the Mossbauer spectra show line broadening and the difference between the 1,6 and 3,4 linewidths is caused by the anisotropic hyperfine field fluctuation. The anisotropic field fluctuation of +H (P$_{+}$=0.80) is greater than -H (P$_{-}$=0.20). We calculated that the anisotropy energy was 124.01 erg/cm$^3$for T=150 K which is associated with the large line broadening.

Crystal Structure and Electrochemical Performance of LiNi1-xCoxO2 (x=0.0~1.0) According to Co Substitution (Co 치환량에 따른 LiNi1-xCoxO2 (x=0.0~1.0)의 결정구조 및 전기화학 특성)

  • Hong, Jin K.;Oh, Seung M.
    • Journal of the Korean Electrochemical Society
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    • v.6 no.1
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    • pp.1-5
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    • 2003
  • [ $LiNi_{1-x}Co_xO_2\;(x=0.0\~1.0)$ ] powders were synthesized by citrate method, and their crystal structures and electrochemical performance as the cathode material in Li secondary batteries were analyzed. X-ray diffraction analysis revealed that all the samples carry a single phase regardless of the Co substitution. The results of Rietveld refinement suggested that the crystal structure of solid solutions varies according to the Co substitution. When the Co substitution is low $(x=0.3\~0.5)$, the solid solutions carry a cubic-like structure with a relatively small value in the ratio of lattice parameters (c/a). The solid solutions made with a higher Co substitution (x=0.7), however, exhibit a layered structure with a higher c/a ratio. This difference was also observed in the electrochemical voltage spectroscopy (EVS) profiles, whereby the Co component in scarcely substituted materials shows a charging reaction at $3.7V\;(vs.\;Li/Li^+)$, but in the heavily substituted ones at 3.92V.

Synthesis, Characterizations, and Applications of Metal-Ions Incorporated High Quality MCM-41 Catalysts (고품질 금속 이온 첨가 MCM-41 분자체 촉매의 제법, 특성화 및 응용 반응)

  • Lim, Steven S.;Haller, Gary L.
    • Korean Chemical Engineering Research
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    • v.51 no.4
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    • pp.443-454
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    • 2013
  • Various metal ions (transition and base metals) incorporated MCM-41 catalysts can be synthesized using colloidal and soluble silica with non-sodium involved process. Transition metal ion-typically $V^{5+}$, $Co^{2+}$, and $Ni^{2+}$-incorporated MCM-41 catalysts were synthesized by isomorphous substitution of Si ions in the framework. Each incorporated metal ion created a single species in the silica framework, single-site solid catalyst, showing a substantial stability in reduction and catalytic activity. Radius of pore curvature effect was investigated with Co-MCM-41 by temperature programmed reduction (TPR). The size of metallic Co clusters, sub-nanometer, could be controlled by a proper reduction treatment of Co-MCM-41 having different pore size and the initial pH adjustment of the Co-MCM-41 synthesis solution. These small metallic clusters showed a high stability under a harsh reaction condition without serious migration, resulting from a direct anchoring of small metallic clusters to the partially or unreduced metal ions on the surface. After a complete reduction, partial occlusion of the metallic cluster surface by amorphous silica stabilized the particles against aggregations. As a probe reaction of particle size sensitivity, carbon single wall nanotubes (SWNT) were synthesized using Co-MCM-41. A metallic cluster stability test was performed by CO methanation using Co- and Ni-MCM-41. Methanol and methane partial oxidations were carried out with V-MCM-41, and the radius of pore curvature effect on the catalytic activity was investigated.

Mossbauer Studies of the $H_2$ Reduction Effects On Magnetic Properties of Sr-Ba Substituted Hexgonal Ferrite (치환형 Sr-Ba 육방 페라이트들의 자기적 성질에 수소환원이 미치는 효과에 관한 Mossbauer 분광학적 연구)

  • 박재윤;권명회;이재광
    • Journal of the Korean Magnetics Society
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    • v.9 no.1
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    • pp.35-40
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    • 1999
  • Sr substituted materials for some barium in M-type barium ferrite powder and Co-Ti substituted Sr-Ba hexagonal ferrite powder were prepared by citrate sol-gel method and 2 MOE sol-gel method these hexaferrite particles were reduced for 1hr in the hydrogen gas. The reduction temperatures were varied in the range of 250 $^{\circ}C$ to 500 $^{\circ}C$. X-ray diffraction patterns were measured using diffractometer with Cu $K_{\Alhpa}$ radiation. Mossbauer absorption spectra were measured with a constant acceleration spectrometer. We have focused on studying the origin of increasing $M_s$ by M$\"{o}$ssbauer spectroscopy. Ferrite particles which were sintered at 105$0^{\circ}C$ were found to be typical magnetoplumbite structure and single phase. XRD patterns with varying the reduction temperatures in $Sr_{0.5}Ba_{0.5}Fe_{10}O_{19}$ indicates ferrites particles become composite hexaferrites containing $\alpha$-Fe at T_{red}=350 \;$^{\circ}C$$. On the otherhand, it was found that $Co^{2+}$ ions and $Ti^{4+}$ ions in $Sr_{0.7}Ba_{0.3}Fe_{10}CoTiO_{19}$ prevent from changing $Fe^{3+}$ ions to $\alpha$-Fe during the $H_2$ reduction. Comparing Mossbauer results with XRD results, we have determined most of $\alpha$-Fe are reduced from $4f_{vi}$ sites and 12k sites of $Fe^{3+}$ ions. These $\alpha$-Fe phase bring the induced anisotropy and increase saturation magnetization $M_s$.TEX>.

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Partial Oxidation of CH4 Using {0.7}Sr0.3Ga0.6Fe0.4O3-δ for Soild Oxide Fuel Cell (고체산화물 연료전지용 La0.7Sr0.3Ga0.6Fe0.4O3-δ계의 메탄부분산화반응)

  • Lee, Seung-Young;Lee, Kee-Sung;Lee, Shi-Woo;Kim, Jong-Won;Woo, Sang-Kuk
    • Journal of the Korean Electrochemical Society
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    • v.6 no.1
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    • pp.59-64
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    • 2003
  • We fabricated mixed ionic-electronic conducting membranes, $CH_4\;Using\;{0.7}Sr_{0.3}Ga_{0.6}Fe_{0.4}O_{3-\delta}$, by solid state reaction method for solid oxide fuel cell. The membranes consisted of single perovskite phase and exhibited high relative density, $>95\%$. We coated $La_{0.6}Sr_{0.4}CoO_{3-\delta}$ layer using screen printing method in order to improve surface reactivity of the $La_{0.7}Sr_{0.3}Ga_{0.6}Fe_{0.4}O_{3-\delta}$. As a result, the oxygen permeation flux of the coated $La_{0.7}Sr_{0.3}Ga_{0.6}Fe_{0.4}O_{3-\delta}$ showed higher value, $0.5ml/min{\cdot}cm^2\;at\;950^{\circ}C$ than the uncoated one. Higher oxygen permeation was observed in the porously coated Lao $La_{0.7}Sr_{0.3}Ga_{0.6}Fe_{0.4}O_{3-\delta}$membranes with larger grain sizes. Syngas, $CO+H_2$, was successfully obtained from methane gas, $CH_4$, using the $La_{0.6}Sr_{0.4}CoO_{3-\delta}$ coated $La_{0.7}Sr_{0.3}Ga_{0.6}Fe_{0.4}O_{3-\delta}$, with over $40\%\;of\;CH_4$ conversion and syngas yield. $La_{0.7}Sr_{0.3}Ga_{0.6}Fe_{0.4}O_{3-\delta}$ membrane was stable even when it was exposed to the reducing environment, methane, for 600 hrs at $950^{\circ}C$.

Study on the Structural and Transporting Property of Sr2Ru1-xCuxO4-y(0.0≤x≤0.5) (Sr2Ru1-xCuxO4-y(0.0≤x≤0.5) 화합물의 구조 및 전달 특성에 대한 연구)

  • Park, Jung-Chul
    • Journal of the Korean Chemical Society
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    • v.47 no.6
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    • pp.614-618
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    • 2003
  • $Sr_2Ru_{1-x}Cu_xO_{4-y}(0.0{\le}x{\le}0.5)$ compounds were prepared using a conventional solid state reaction. Based on the Rietveld refinements of X-ray diffraction results, it is revealed that $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds are the single phases with K2NiF4 type tetragonal system in the range of 0=x=0.3, while the mixed phases of$Sr_2RuO_4$ and $Sr_2CuO_3$ in the range of $0.4{\le}x{\le}0.5$. By means of X-ray photoelectron spectroscopy, the valence states of Ru and Cu in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, have been confirmed to 4+ and 2+, respectively. The bond length difference between $Ru-O_1 ({\times}4)\;and\;Ru-O_2 ({\times}2)\;in\;RuO_6$ octahedron is gradually decreased with increasing Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, which results in the lower c/a ratio. So, it might be assured that the variation of local symmetry of $RuO_6$ octahedron is very closely related to the transporting property of $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds. The behavior of resistivity discloses that the metallic property in $Sr_2RuO_4$ changes into the semiconducting one in proportion to the Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$.

Purification and Cellular Localization of Extracellular Nuclease of Serratia marcescens Expressed in Escherichia coli (대장균에 발현된 Serratia marcescens의 Nuclease의 정제와 세포내 분포)

  • Kim, Woe-Yeon;Lee, Hoon-Sil;Suh, Sook-Jae;Cho, Moo-Je;Lee, Sang-Yeol;Kim, Jae-Won
    • Korean Journal of Microbiology
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    • v.32 no.2
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    • pp.147-154
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    • 1994
  • Nuclease was secreted to the environmental media from the Escherichia coli JM107 tranformant harboring the extracellular nuclease gene of Serratia marcescens in the plasmid of pNUC4. Under the growth conditions, the amount of secreted enzyme was increased in parallel with bacterial growth conditions, the amount of secreted enzyme was increased in parallel with bacterial growth. The enzyme was purified using chromatofraphic procedures of Matrex green gel and heparin agarose affinity gel, resulted in 50-fold purification with 15% recovery of the enzyme. The apparent molecular weight of the enzyme was estimated to be 29Kda by sodium dodecylsulfate denaturing gel electrophoresis. Using the purified enzyme, polyclonal antibody was obtained from the rabbit. The specificity of the antibody was confirmed by immunoblotting and immunoprecipitaion. For the investigation of cellular distribution of the enzyme, cells were fractionated into three fractions; cytoplasm, periplasm and extracellular fluid. While more than 80% of the enzymatic activity was detected in the extracellular fluid and periplasm, a little was found in the cytoplasm, indicating that the enzyme was likely to be immediately exported to the membrane for excretion after biosynthesis. These results were confirmed again by immunocytochemistry technique using the antibody.

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Dielectric Properties and Ordering Structures of Pb(Fe1/2Ta1/2)O3-Pb(Fe1/2Nb1/2)O3 Solid Solutions (Pb(Fe1/2Ta1/2)O3-Pb(Fe1/2Nb1/2)O3 고용체의 유전특성 및 질서배열구조)

  • Woo, Byong-Chul;Kim, Byung-Kook;Lee, Jong-Ho;Park, Hyun-Min;Kim, Byong-Ho
    • Journal of the Korean Ceramic Society
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    • v.39 no.9
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    • pp.863-870
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    • 2002
  • The Single phase $Pb(Fe_{1/2}Ta_{1/2})O_3$ (x=0.0∼1.0) solid solutions were successfully synthesized and their ordering structures as well as dielectric properties were investigated ${{r(Nb^{5+})=r(Ta^{5+})=0.78 {\AA},\;AW(Nb^{5+})=92.91,\;AW(Ta^{5+})=180.95}}$. While $Pb(Fe_{1/2}Ta_{1/2})O_3$ showed typical relaxor ferroelectric characteristics such as dielectric relaxation and diffuse phase transition, the sharpeness of the phase transition increased as $Ta^{5+}$ was replaced by $Nb^{5+}$ and finally $Pb(Fe_{1/2}Nb_{1/2})O_3$ showed normal ferroelectric characteristics with no dielectric relaxation. By using Raman spectroscopy, it was revealed that the $Fe^{3+}\;and\;Ta^{5+}\;of\;Pb(Fe_{1/2}Ta_{1/2})O_3$ were stoichiometrically 1:1 ordered within the short range which can be hardly probed even by TEM. Also, The degree of ordering in $Pb(Fe_{1/2}Ta_{1/2})O_3$ decreased as $Ta^{5+}$ was replaced by $Nb^{5+}$ and finally $Fe^{3+}\;and\;Nb^{5+}\;of\;Pb(Fe_{1/2}Nb_{1/2})O_3$ were completely disordered. The relaxor ferroelectric characteristics of $Pb(Fe_{1/2}Ta_{1/2})O_3$ could be correlated with the stoichiometric 1:1 ordering of B-site cations within the short range which can be hardly probed even by TEM. Also, the decrease of the relaxor ferroelectric characteristics with the replacement of $Ta^{5+}\;by\;Nb^{5+}$ could be correlated with the weakening of the ordering and the normal ferroelectric characteristics of $Pb(Fe_{1/2}Nb_{1/2})O_3$ could be correlated with the complete disordering of B-site cations.