• Title/Summary/Keyword: 중성자분말회절법

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온도증가에 따른 삼팔면체운모 내 OH기의 구조변화 연구; 중성자 분말회절법을 이용한 In-situ 연구

  • 이철규;송윤구;김신애;문희수;전철민;성기훈
    • Proceedings of the KSEEG Conference
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    • 2003.04a
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    • pp.175-177
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    • 2003
  • 삼팔면체 운모의 결정구조에 대한 연구는 많은 학자들에 의해 진행되어 왔다. 하지만 주로 X선 단결정법을 이용하였기 때문에 수소에 대한 정보는 부족하다. 온도의 증가나 풍화에 의해 결정구조의 변화는 수산화기의 길이나 방향성에 영향을 주는데 위와 같은 X선에 의한 연구로는 한계를 가지게 된다. 이러한 단점을 극복하기 위한 방법으로 중성자 단결정법이나 중성자분말회절법을 사용할 수 있으나 중성자 단결정법은 일정크기 이상($5{\times}5{\times}0.4$mm, Rayner 1974)의 완전한 단결정을 대상시료로 이용해야 하는 단점이 있다. (중략)

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The Rietveld Structure Refinement of Natural Phlogopite Using Neutron Powder Diffraction (중성자분말회절법을 이용한 금운모 결정에 대한 리트벨트 구조분석)

  • 이철규;송윤구;전철민;김신애;성기훈
    • Journal of the Mineralogical Society of Korea
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    • v.16 no.3
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    • pp.215-222
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    • 2003
  • The Rietveld structure refinement for the natural trioctahedral mica, phlogopite-1M (Parker Mine, Quebec, Canada) has been done by high resolution neutron powder diffraction at $25^{\circ}C$ and -263$^{\circ}C$. The structural formula of phlogopite determined by electron probe microanalysis is $K_2$(M $g_{4.46}$F $e_{0.83}$A $l_{0.34}$ $Ti_{0.22}$)(S $i_{5.51}$A $l_{2.49}$) $O_{20}$(O $H_{3.59}$ $F_{0.41}$). Cell parameters are a=5.30∼5.31 $\AA$, b=9.18∼9.20 $\AA$, c=10.18∼10.21 $\AA$, $\beta$=100.06∼100.08$^{\circ}$. Refinements converged to R values in the range of $R_{p}$=2.35%, $R_{wp}$=3.01%, respectively. In this study, the OH bond length is calculated to 0.93 $\AA$ at room temperature and 1.03 $\AA$ at -263$^{\circ}C$, and the angles between OH vector and (001) plane are obtained 93.4$^{\circ}$∼93.6$^{\circ}$. The decrease in the length of OH with the increase in temperature should be due to the hydrogen bonding in the structure of phogopite.e.e.f phogopite.e.e.

Amorphization Process Induced by mechanical Alloying under N2 Gas Atomosphere in Cu-V and Fe-Cr System. (질소가스 분위기 중 기계적 합금화에 의한 Cu-V 및 Fe-Cr 계의 비정질화 과정)

  • Lee, Chung-Hyo
    • Korean Journal of Materials Research
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    • v.6 no.8
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    • pp.796-800
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    • 1996
  • 질소가스 분위기 중에서 Cu30V70 및 Fe30Cr70 혼합분말을 기계적 합금화 (MA)처리한 결과, 두 합금계에서 비정질화가 관찰되었다. 결정질에서 비정질상으로의 구조변화 과정을 Xtjs 회절 및 중성자 회절법에 의해 관찰되었다. 결정질에서 비정질상으로의 구조변화 과정을 X선 회절 및 중성자 회절법에 의해 관찰하였다. 그 결과, 이 합금계에서의 비정질화는 각 결정구조에서 전형적으로 존재하는 8면체 unit가 선택적으로 붕괴되어 4면체 unit로 변화되어 가는 과정임을 알 수 있었다. 또한, 중성자회절 결과로부터 질소원자는 금속원자로 이루어진 4면체의 중심에 위치하고 있음을 알 수 있었다.

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Neutron Diffraction Study on the Crystal Structure of Yttria-Stabilized Zirconium Oxide (중성자회절법을 이용한 이트리아 저코니아의 결정구조 연구)

  • Jin-Ho Lee;Chang-Hee Lee;Won-Sa Kim
    • Journal of the Mineralogical Society of Korea
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    • v.13 no.3
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    • pp.164-170
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    • 2000
  • Neutron single crystal and powder diffraction techniques have been applied to the structure analysis of yttria-stabilized zirconium, Z $r_{0.73}$ $Y_{0.27}$ $O_{1.87}$., prepared by the skull-melting method. The crystal structure has been determined to be cubic symmetry, space group Fm/equation omitted/ with a=5.155(2)$\AA$, V=136.99(5)$\AA$, Z=4, and R(F)=5.65%, $\omega$R(I)=10.57% for 70 integrated intensities of Bragg Peaks observed from single crystal of Z $r_{0.73}$ $Y_{0.27}$ $O_{1.87}$. The stabilizer atoms randomly occupy the zirconium sites and there are displacements of oxygen atoms with amplitudes of $\Delta$/a~0.033 and 0.11 along <110> and <100> directions from the ideal positions of the fluorite structure, respectively. There are no significant differences in crystallographic data between the single crystal and powder studies. Diffraction pattern after Rietveld refinement, using neutron powder data, has shown the evidence of a tetragonal impurity phase, or a slight tetragonal distortion.

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Phase Analysis of Mechanically Alloyed $\sigma$-VFe Alloy Powders by Neutron and X-ray Diffraction (기계적 합금화한 $\sigma$-VFe합금의 중성자 및 X선 회절에 의한 상분석)

  • 이충효;조재문;이상진;심해섭;이창희
    • Korean Journal of Materials Research
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    • v.11 no.8
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    • pp.664-664
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    • 2001
  • The mechanical alloying (MA) effect in $\sigma$-VFe intermetallic compound was studied by neutron and X-ray diffraction. The structure of MA $\sigma$-VFe powders were characterized by the X- ray diffraction with Cu- $K\alpha$ radiation and neutron diffraction with monochromatic neutrons of $1.835\AA$ using a high resolution powder diffractometer (HRPD). Mechanical alloying of $\sigma$-VFe compound gives rise to a dramatic structural change. After 60 hours of MA, the Fe-Fe distribution of the $\sigma$- phase VFe tetragonal structure with 30 atoms in a unit cell is found to change into that of the $\sigma$-(V,Fe) solid solution with bcc structure, which is a stable phase at elevated temperature above $1200^{\circ}C$. A comparison of X-ray diffraction data for the $\alpha$-phase has been also made with the corresponding neutron diffraction data. The (101) and (111) diffraction peaks of the $\sigma$-phase was clearly observed only in neutron diffraction pattern, which is believed to be a characteristic feature due to the chemical atomic ordering of $\sigma$- VFe phase.

Mechanical alloying effect and structural observation of (V, Fe)-N amorphous alloy powders (기계적 합금화에 의한 (V, Fe)-N계 비정질 합금의 제조 및 구조변화)

  • 이충효;전성용;김지순
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.4
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    • pp.129-134
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    • 2004
  • In this study, we investigated the effect of a nitrogen atom on the amorphization of V-Fe alloy through solid-gas reaction during mechanical alloying (MA). MA by planetary ball mill of $V_{70}Fe_{30}$ elemental powders was carried out under the nitrogen gas atmosphere. Amorphization has been observed after 160 hours of ball milling in this case. The DSC spectrum for the mechanically alloyed ($V_{70}Fe$_{30}$)_{0.89}N_{0.11}$ powders exhibits a sharp exothermic peak due to crystallization at about $600^{\circ}C$. Structural transformation from the bcc crystalline to amorphous states was also observed through X-ray and neutron diffractions. We take a full advantage of a negligibly small scattering length of the V atom in the neutron diffraction measurement. During amorphization process the octahedral unit, which is typical of a polyhedron formed in any crystal structures, was preferentially destroyed and transformed into the tetrahedral unit. Futhermore, neutron diffraction measurements revealed that a nitrogen atom is selectively situated at a center of the polyhedron formed by V atoms.

A study on neutron diffraction of amorphous Ni-Ta and Cu-Ta alloy powders prepared by mechanical alloying (기계적 합금화법으로 제조한 비정질 Ni-Ta 및 Cu-Ta 합금분말의 중성자회절에 관한 연구)

  • Lee, Chung-Hyo;Lee, Jin
    • Electrical & Electronic Materials
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    • v.8 no.6
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    • pp.715-720
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    • 1995
  • 기계적 합금화법에 의한 비정질화 과정을 Ni-Ta계 및 Cu-Ta계에 대하여 조사하였다. Ni-Ta합금계는 혼합엔탈피가 음이나, Cu-Ta계는 혼합엔탈피가 양인 열역학적으로 대조적인 합금계이다. 볼밀 중 발생하는 원자구조 변화를 중성자회절법을 이용하여 관찰하였다. 두 합금게에 있어서 기계적 합금화에 의한 비정질상이 생성되었다. 비정질 Cu-Ta합금의 local원자구조를 혼합엔탈피가 크게 음인 Ni-Ta계의 결과와 비교하였다. 그 결과, 대조적 특성을 가진 두 합금계임에도 불구하고 원자크기가 작은 Ni 및 Cu가 bcc Ta의 결정격자 속으로 우선적으로 침입함으로써 비정질화가 진행됨을 알 수 있었다.

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Synthesis of amorphous Fe-Cr-N alloy powders by mechanical alloying (기계적 합금화에 의한 Fe-Cr-N 계 비정질 합금분말의 제조)

  • 이충효
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.1
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    • pp.132-136
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    • 1999
  • Mechanical alloying (MA) by ball mill of $Fe_{30}Cr_{70}$ elemental powders was carried out under the nitrogen gas atmosphere. Amorphization has been observed in this case, while MA under an inert argon gas atmosphere produces the bcc solid solution. The DSC spectrum for the mechanically alloyed $(Fe_{30}Cr_{70})_{0.85}N_{0.15)$powders exhibits a sharp exothermic peak due to crystallization at about $550^{\circ}C$. Structural transformation from the bcc crystalline to amorphous states was observed through X-ray and neutron diffractions. During amorphization process the octahedral unit, which is typical of a polyhedron formed in any crystal structures, was preferentially destroyed and transformed into the tetrahedral unit. Futhermore, neutron diffraction measurements revealed that a nitrogen atom is situated at a center of the tetrahedron formed by metal atoms.

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