• Title/Summary/Keyword: X-선 구조분석

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Crystallographic and Magnetic Properties of a Perovskite La1/3Sr2/3FeO2.96 (페롭스카이트 La1/3Sr2/3FeO2.96의 결정학적 및 자기적 성질에 관한 연구)

  • Yoon, Sung-Hyun
    • Journal of the Korean Magnetics Society
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    • v.15 no.3
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    • pp.167-171
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    • 2005
  • Detailed aspects of the charge disproportionation (CD) transition for a polycrystalline $La_{1/3}Sr_{2/3}FeO_{2.96}$ were studied with the X-ray diffraction, $M\ddot{o}ssbauer$ spectroscopy, and SQUID magnetometer. The crystal structure was found to be rhombohedral with a space group R/3c. The lattice parameters were $a_R=5.4874\;\AA,\;and\;a_R=60.07^{\circ}$, respectively. $M\ddot{o}ssbauer$ spectra were taken within a wide range of temperature from 4.2 K up to room temperature. In the low temperature region, the spectra were comprised of two superimposed sextets which originated from $Fe^{3+}\;and\;Fe^{5+}$, respectively. This was the antiferromagnetic mixed valence state produced by the charges disproportionated into two different species. In the high temperature region, however, only a singlet from $Fe^{3.6+}$ was observed, indicating that it was a paramagnetic averaged valence state. The CD transition occurred in the temperature range from 175 K to 200 K, in which the two phases coexisted. The origin for the CD transition was explained by the thermally generated fast hopping of electrons. Hysteresis loop showed that there existed a strong antiferromagnetic interaction among magnetic ions. As the temperature increased thru the CD transition temperature, it was very likely that the interaction between $Fe^{3+}\;and\;Fe^{5+}$ was replaced by a more stronger one.

Preparation of nanocrystalline $TiO_2$ photocatalyst films by using a titanium naphthenate (티타늄 나프테네이트를 이용한 나노결정질 $TiO_2$ 광촉매 박막의 제조)

  • 이선옥;김상복;윤연흠;강보안;황규석;오정선;양순호;김병훈
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.12 no.5
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    • pp.240-246
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    • 2002
  • $TiO_2$ films on soda-lime-silica glasses were prepared by spin coating-pyrolysis process using titanium naphthenate as a starting material. As-deposited films were pyrolyzed at $500^{\circ}C$ for 10 min in air and annealed at 500, 550 and $600^{\circ}C$ for 30 min in air. Crystallinity of the film was investigated by X-ray diffraction analysis. A field emission-scanning electron microscope and an atomic force microscope were used for characterizing the surface morphology and the surface roughness of the film. After annealing at 550 and $600^{\circ}C$, the X-ray diffraction patterns consist of only anatase peak. Films annealed at 500 and $550^{\circ}C$ exhibited flat surfaces. While with the increase in annealing temperature to $600^{\circ}C$, the $TiO_2$ film showed abnormal growth of three-dimensional needle-shaped grains. For all samples, high transmittance, above 90 % at 500 nm, was obtained at visible range. To investigate photocatalytic properties, IR absorbance associated with the C-H stretching vibrations of a thin solution-cast film of stearic acid under 365 nm (2.4 mW/$\textrm{cm}^2$) UV irradiation was estimated.

A study on the delectric and piezoelectric properties of the Pb($Zn_{1}$3$Nb_{2}$3/)$_{3}$-Ba($Zn_{1}$3/$Nb_{2}$3/)$P_{3}$-PbT$iO_{3}$ ceramics (Pb($Zn_{1}$3/$Nb_{2}$3/)$O_{3}$-Ba($Zn_{1}$3/$Nb_{2}$3)$O_{3}$ - PbT$iO_{3}$ 세라믹의 유전 및 압전특성에 관한 연구)

  • 박혜옥;이성갑;배선기;이영희
    • Electrical & Electronic Materials
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    • v.3 no.3
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    • pp.233-241
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    • 1990
  • 본 연구에서는 xPb(Zn$_{1}$3/Nb$_{2}$3/)O$_{3}$-yBa(Zn$_{1}$3/Nb$_{2}$3/)O$_{3}$-zPbTiO(0.50.leq.x.leq.0.60, 0.10.leq.y.leq.0.20, 0.20.leq.z.leq.0.40)세라믹을 1050.deg.C에서 2시간동안 유지시켜 일반소성법으로 제작하였다. 시편 제작시 조성은 조성변태 상경계부근을 선택하였으며 Ba(Zn$_{1}$3/ Nb$_{2}$3/)O$_{3}$ 고용량에 따른 purochlore상의 억제 및 그 영향을 조사하고 구조적, 유전적 및 압전적 특성을 측정하였다. X-선 회절분석 및 미세구조의 관찰 결과, Ba(Zn$_{1}$3/Nb$_{2}$3/)O$_{3}$의 고용량에 따라 pyrochlore상 및 미반응 물질등은 억제되어 0.20mol 고용된 시편에서는 균질한 perovskite상이 형성되었다. Ba(Zn$_{1}$3/Nb$_{2}$3/)O$_{3}$의 고용량이 증가함에 따라 유전상수는 증가하여 0.50PZN-0.20BZN-0.30PT시편의 경우 6880.9의 높은 값을 나타내었으며 정전용량의 온도계수는 감소하여 0.383[%/.deg.C]의 양호한 값을 나타내었다. 큐리온도는 PbTiO$_{3}$의 고용량이 0.20mol에서 0.40mol로 증가함에 따라 30.deg.C에서 170.deg.C로 증가하였다. 전기기계 결합계수 (K$_{p}$), 기계적 품질계수(Qm) 및 압전전하 계수 (d$_{33}$)는 조성변태 상경계 부근의 조성에서 크게 나타났으며 0.60PZN-0.15BZN-0.25PT 시편의 경우 각각 58.5%, 120.5, 150x$10^{-12}$[C/N]의 값을 나타내었다.다.다.

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Evolution of Metastable $L1_2-Al_3(Nb_xZr_{1-x})$ Phases in Rapidly Quenched Al-Nb-Zr Alloys

  • Park, Min-Woo
    • Journal of Korea Foundry Society
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    • v.27 no.6
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    • pp.250-254
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    • 2007
  • 3원계 Al-Nb-Zr의 용응 합금을 스프렛 ?봬?(splat-quenching) 방법을 이용하여 급속냉각응고 한 후, 응고된 시편을 698K에서 200시간까지 열처리하여 상전이를 연구하였다. 급속응고 및 열처리된 시편의 미세구조는 X-선 회절 및 투과전자 현미경으로 분석하였다. Al-1.95Nb-0.65Zr, Al-1.3Nb-1.3Zr, 및 Al-0.65Nb-1.95Zr (at%) 3원 합금계를 연구하였다. 각 합금의 조성은 Vegard's 법칙을 적용하여 Al(${\alpha}$)의 기지조직과 $L1_2-Al_3(Nb,Zr)$의 석출상들이 정합을 이루도록 선택되었다. 급속응고된 후 각 합금은 과고용된 Al(${\alpha}$)의 고용상을 형성하였다. Al-1.3Nb-1.3Zr, 및 Al-0.65Nb-1.95Zr의 급속응고된 상태의 시편을 698K에서 열처리하여 알루미늄 기지와 정합의 계면을 갖는 $L1_2-Al_3(Nb_{0.5}Zr_{0.5})$$L1_2-Al_3(Nb_{0.25}Zr_{0.75})$의 상을 각각 석출하였다. 반면 Al-1.95Nb-0.65Zr 합금은 평형상인 $D0_{22}-Al_3(Nb_{0.75}Zr_{0.25})$ 상을 석출하였다. 준안정상의 정합 $Al_3(Nb,Zr)$ 미세 분산상 석출은 입자의 조대화를 억제하고 재료의 고온 강도를 증가될 것으로 사료된다.

Crystallographic and Magnetic Properties of KFeO2 (KFeO2 분말의 제조 및 뫼스바우어 분광학 연구)

  • Moon, Seung-Je;Shim, In-Bo;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.38-42
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    • 2007
  • The crystallographic and magnetic properties of $KFeO_2$ powder prepared by ball-mill method, have been studied by x-ray diffraction(XRD), $M\"{o}ssbauer$ spectroscopy, and vibrating sample magnetometer(VSM) measurements. The crystal structure of $KFeO_2$ powder at room temperature is determined to be an orthorhombic structure of Pbca with its lattice constants $a_0=5.557{\AA},\;b_0=11.227{\AA},\;c_0=15.890{\AA}$ by Rietveld refinement. $M\"{o}ssbauer$ spectra of $KFeO_2$ were taken at various temperatures ranging from 4.2 to 818 K. The magnetic hyperfine field and isomer shift value at 4.2 K and RT were 519 kOe, 489 kOe and 0.19 mm/s, 0.05 mm/s respectively. The average hyperfine field $H_{hf}(T)$ of the $KFeO_2$ shows a temperature dependence of $[H_{hf}(T)-H_{hf}(0)]/H_{hf}(0)=-0.36(T/T_N)^{5/2}$ for $T/T_N$<0.7, indicative of spin-wave excitation.

Micromorphology and Chemical Composition of a Sialolith in the Submandibular Gland Duct (악하선 내 타석의 미세형상 및 화학적 조성)

  • Im, Yeong-Gwan;Song, Ho-Jun;Kim, Byung-Gook
    • Journal of Oral Medicine and Pain
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    • v.36 no.3
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    • pp.161-167
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    • 2011
  • Sialolith is one of the most common pathologic conditions found in the salivary glands. The mechanisms responsible for the formation of sialoliths have not been elucidated so far. In this article, the chemical composition and micromorphology of a sialolith of a 58-year old female patient suffering from chronic sialoadenitis of the submandibular gland was analyzed using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). In a SEM evaluation, the highly mineralized amorphous core surrounded by lamellar and concentric structures was revealed, however no foreign body, organic material, or signs of microorganism were observed in the core of the sialolith. EDX analysis showed the central core was composed of only Ca, O and P, and that a high level of C was detected near the central area as well. These results indicated that the inorganic composition of the sialolith was hydroxyapatite crystals, and that inorganic and organic substances existed around the central cores. This study suggests that the sialolith was composed mainly of hydroxyapatite crystals and the formation of the nucleus of the sialolith in the submandibular gland duct was secondary to sialadenitis, which favors the growth of an inorganic crystalline nucleus.

Preparation and crystal structure of azido bridged one-dimensional polymeric cadmium(II) complex, [Cd(N3)2(2-ethylimidazole)2]

  • Suh, Seung Wook;Kim, Inn Hoe;Kim, Chong-Hyeak
    • Analytical Science and Technology
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    • v.18 no.5
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    • pp.391-395
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    • 2005
  • The title complex, $[Cd(N_3)_2(2-ethylimidazole)_2]$, I, has been prepared and characterized by X-ray single crystallography. The complex I crystallizes in the monoclinic system, Cc space group with a = 16.200(3), b = 12.926(3), $c=7.007(1){\AA}$, ${\beta}=102.29(3)^{\circ}$, $V=1433.7(5){\AA}^3$, Z = 4, $R_1=0.0239$ and ${\omega}R_2=0.0604$ for 1874 independent reflections. Cd(II) atom has a slightly distorted octahedral coordination geometry, with four end-on (${\mu}-1$,1) bridging azido ligands and two 2-ethylimidazole ligands bonding through nitrogen atom. The central cadmium(II) atoms are run in parallel to the c-axis and are doubly bridged with neighboring cadmium(II) atoms by the end-on (${\mu}-1$,1) bridging azido ligands. Thus, this complex has a one-dimensional zigzag chain structure in which the 2-ethylimidazole is in the cis conformation.

Performance Test of 4Cl Beamline for Protein Solution Scattering at the PLS (용액상의 단백질 구조 분석을 위한 PLS 4Cl빔라인의 성능 테스트)

  • Yu Chung-Jong;Kim Jehan;Kim Kwang-Woo;Kim Ghyung-Hwa;Lee Heung-Soo;Ree Moonhor;Kim Kyung-Jin
    • Journal of the Korean Vacuum Society
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    • v.14 no.3
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    • pp.138-142
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    • 2005
  • We tested performance of the 4C1 beamline for analyzing structures of proteins in solution using small angle X-ray scattering (SAXS) at the Pohang Light Source(PLS). Structurally well-known proteins such as lysozyme and $Bcl-XL(\vartriangle TM/\vartriangle loop)$ were used for the study. Low resolution solution structures of lysozyme and $Bcl-XL(\vartriangle TM/\vartriangle loop)$ were obtained at a resolution of at least i.2 nm, and the structures were basically same as those calculated from the crystal structures of the proteins. We also used $Bcl-XL(\vartriangle TM/\vartriangle loop)$ with a long flexible loop attached [$Bcl-XL(\vartriangleTM))$] and obtained significantly different data from $Bcl-XL(\vartriangle TM/\vartriangle loop)$, although the electron density map of the loop is known to be invisible from the crystal structure of $Bcl-XL(\vartriangleTM))$. We confirm that SAXS experiment is a powerful tool for the structural study of proteins in solution and the 4Cl beamline at the PLS is well-equipped and suitable for the protein solution SAXS experiment.

Basic Study on P(VDF-TrFE) Smart Sensor for Monitoring Composite Structure Behaviors (복합재료구조물 거동 관찰을 위한 P(VDF-TrFE) 스마트센서의 기초연구)

  • Bae, Ji-Hun;Chang, Seung-Hwan
    • Composites Research
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    • v.28 no.3
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    • pp.75-80
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    • 2015
  • Poly(vinylidene fluoride-trifluoroethylene; P(VDF-TrFE)) is one of the most promising electroactive polymers with numerous application potentials in many fields of industry. Because of its good electro-mechanical properties P(VDF-TrFE) has been used for a number of sensors and actuators and also can be used for monitoring composite structure behaviors as a sensor. Three different ways (Electrical poling, annealing-cooling, and pressing) to enhance ${\beta}$-phase of P(VDF-TrFE) film were carried out. A microscopic analysis was conducted using X-ray diffraction to investigate the effect of such treatments on piezoelectric properties of P(VDF-TrFE) film. From the results, poling, annealing-cooling, and pressing were all effective to enhance ${\beta}$ crystallinity of P(VDF-TrFE) film and the maximum increase rate was 62.80% from 45.29% of the control group.

Preparation of $Pb(Sc_{1/2}Nb_{1/2})O_3$ powders by the molten salt synthesis method (용융염 합성법에 의한 $Pb(Sc_{1/2}Nb_{1/2})O_3$ 분말의 제조)

  • 박경봉
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.3
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    • pp.400-405
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    • 1997
  • Lead scandium niobate powders were prepared by a molten salt synthesis method using KCl as a flux. Variations in phase formation and particle morphology were investigated for the temperature range $700^{\circ}C$ to $850^{\circ}C$. Pure $Pb(Sc_{1/2}Nb_{1/2})O_3$ perovskite phase was formed at $850^{\circ}C$ after 2hrs and the average particle size of powder was below 0.5 $\mu\textrm{m}$. The results are discussed with respect to DTA, X-ray diffraction, and microstructural characterization data.

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