• Title/Summary/Keyword: Rietveld method.

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Hydraulic Reaction Analysis of C3A in Ordinary Portland Cement with Mineral Additions by Rietveld Method (리트벨트법에 의한 혼합재 첨가 보통 포틀랜드 시멘트 중 C3A 수화반응 해석)

  • Lim, Young-Jin;Lee, Seung-Heun;Cho, Jae-Woo
    • Journal of the Korean Ceramic Society
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    • v.51 no.2
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    • pp.82-87
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    • 2014
  • Due to the revised Korean standard KS L 5201 for Ordinary Portland Cement (OPC), the use of mixed cement has grown from 5% to 10%. This study investigates the hydration behavior of $C_3A$, asit is a cement mixture that is more commonly used than granulated blast furnace slag or limestone alone. Paste samples were prepared with either granulated blast furnace slag or limestone alone. Each sample was compared with the widely used Rietveld method with a cement mixture containing blast furnace slag or limestone. The hydration behavior of $C_3A$ in each OPC sample was assessed and results were analyzed. Granulated blast furnace slag promotes a high initial level of ettringite, but as the days passed, it promotes an increase in monosulfate, leading to cracks and expansion due to the penetration of sulfates in the solution. However, when limestone is added to the mixture, a transformation of ettringite to monosulfate occurs in the presence of the $CaCO_3$ in the limestone. It is considered that this produces hemi-carbonate and mono-carbonate and thus maintains the ettringite level.

Quantitative Analysis of Rietveld Method Minerals by Sintering Temperature of Cement Clinkers with Fly Ash (리트벨트법에 의한 석탄재를 적용한 시멘트 클링커의 소성 온도별 광물 정량분석)

  • Yoo, Dong-Woo;Im, Young-Jin;Park, Tae-Gyun;Lee, Chang-Hyun
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.8 no.4
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    • pp.514-519
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    • 2020
  • In this study, cement clinkers were sintered at each temperature by replacing some of the clay components of cement clinkers with coal materials. The mineral phase change of sintered cement clinker was quantitatively analyzed by XRD-Rietveld method. As the sintering temperature of cement clinker increased, the amount of belite decreased, the amount of alite increased, and the amount of free-CaO decreased. The form of alite and belite could be distinguished at sintering temperature of 1450℃ or higher. The crystal size was greatly increased at 1500℃ sintering. It was confirmed that the excessive sintering was progressed. Free-CaO decreased with the increase of sintering temperature. At 1450 ℃ or higher, it was less than 0.5%. In 1450℃ or greater, it is determined that enough sintering is included. Therefore, the application of fly ash as a raw material of cement clinker was judged to be usable as a source of chemical components of alumina and iron raw materials.

Structure Refinement of $Nd_3Ba_5Co_4O_{15}$ Phase by Rietveld Method (Rietveld법에 의한 $Nd_3Ba_5Co_4O_{15}$상의 정밀화)

  • 이재열;송수호
    • Korean Journal of Crystallography
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    • v.9 no.1
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    • pp.48-52
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    • 1998
  • The new Nd3Ba5Co4O15 phase was synthesized with Nd2O3, BaCO3, and Co3O4 by solid state reaction at 1200℃ with intermittent grinding. The crystal structure of Nd3Ba5Co4O15 has been refined on X-ray diffraction powder data by means of Rietveld method. The starting model was based on the Nd3.43Ba4.42Co2.23Al1.77O15 structure. The crystal system was hexagonal, space group P63mc(186), a=11.629(3) Å, c=6.842(2) Å. Final R values were Rwp=0.097 and Rp=0.068. The structure consists of clusters of CoVICoIV3O15 in which a CoVI octahedron shares corners with 3CoIV tetrahedra.

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Crystal Structures of Ba-ferrites Synthesize by Coprecipitation-Oxidation Method (공침-산화법으로 합성된 바륨페라이트의 결정구조)

  • 신형섭
    • Journal of the Korean Ceramic Society
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    • v.34 no.10
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    • pp.1045-1052
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    • 1997
  • Barium ferrites (BaFe12O19) were synthesized at the various temperature by the coprecipitation-oxidation method. X-ray diffraction Rietveld analysis for barium ferrites were performed, their microstructures were observed and their magnetic properties were measured, in order to analyze the crystal structures and determine the optimal temperature of heat-treatment. The barium ferrite, its average particle size 80 nm, was formed at 600℃ through the hematite (α-Fe2O3), but the site occupations of the Fe's in tetrahedral and bipyramidal sites and of the Ba relatively low. Increasing the heating temperature, these occupations and the magnetization increased, and the crystal c-axis decreased. These changes were very small at the heat treatment of above 800℃, but the particles were rapidly grown. It is suggested that the optimal temperature of heat-treatment is 800℃, at which temperature crystal structure is relatively stable and the particles hardly ever grow.

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Rietveld Refinement of Oxysulfide $LiAl_{0.24}Mn_{1.76}O_{4-y}S_y (y=0, 0.02)$ Spinel Materials

  • Park, Hyun-Min;Y.K Cho;Sun, Yang-Kook
    • Korean Journal of Crystallography
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    • v.14 no.2
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    • pp.110-114
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    • 2003
  • LiAl/sub 0.24/Mn/sub 1.76/O/sub 4-y/S/sub y/ (y=0, 0.02) were synthesized by the sol-gel method. Both structures were refined by Rietveld method, its structure refined as a cubic spinel, space group Fd-3m, a=8.17937(30) Å and 8.18331(19) Å respectively. Though it has been made a charge/discharge experiment above 20 times, there was no change of 3 V/4 V capacity degradation. It was considered that the volume change of MnO/sub 6/ octahedron induced by sulfur substitution plays a key role in keeping the 3 V/4 V capacity. The refined composition of the compound could be confirmed with the ICP analysis.

Syntheses and Characteristics of $Ln_xCa_{2-x}MnO_4$ {Ln=Gd, Nd, Pr, Sm} ($Ln_xCa_{2-x}MnO_4$ 상의 합성과 특성에 관한 연구 {Ln=Gd, Nd, Pr, Sm})

  • Seo, Sang-Il;Lee, Jai-Yeoul
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.05b
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    • pp.196-199
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    • 2000
  • Since the reports of CMR(colossal magnetoresistance) effects in some single crystal R-P phase $La_{1+x}Sr_{2-x}Mn_2O_7$, considerable researches have been carried out to find optimum composition and to understand the role of dimensionality in the CMR mechanism of this system. In this study, layered perovskite $Ln_xCa_{1-x}MnO_{4}$ (x=0.5, Ln=Pr, Nd, Sm, Gd) phases were synthesized by solid state reaction and their structures were refined by Rietveld method. Electrical and magnetic properties were measured between room temperature and liquid helium temperature and compared with those of two dimensional $La_{1.4}Sr_{1.6}Mn_2O_7$ phase.

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Syntheses and structure refinement of $Ln_{x}MnO_{4}$ {Ln=Gd, Nd, Pr, Sm} ($Ca_{2-X}-Ln_{x}MnO_{4}$상의 합성과 결정구조 정밀화 {Ln=Gd, Nd, Pr, Sm})

  • 서상일;이재열
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.07a
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    • pp.726-729
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    • 2000
  • Though L $a_{1+x}$S $r_{2-x}$M $n_2$ $O_{7}$ n=2 R-P phases have been well known to have CMR effect, it was generally believed that n=1 phase was insulating. But recently monolayered perovskite $Ca_{2-x}$L $n_{x}$Mn $O_4$phase has been reported to show magnetoresistance. In this study, layered perovskite $Ca_{2-x}$L $n_{x}$Mn $O_4$ (x=0, 0.5, Ln=Pr, Nd, Sm, Gd) phases were synthesized by solid state reaction and their structures were refined by Rietveld method. The space groups of $Ca_2$Mn $O_4$, N $d_{0.5}$C $a_{1.5}$Mn $O_4$phases were refined as C2cb and Fmmm, respectively.y.ely.y.y.y.y.y.y.

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Microstructural analysis of the single crystalline AlN and the effect of the annealing on the crystalline quality (단결정 AlN의 미세구조 분석 및 어닐링 공정이 결정성에 미치는 영향)

  • Kim, Jeoung Woon;Bae, Si-Young;Jeong, Seong-Min;Kang, Seung-Min;Kang, Sung;Kim, Cheol-Jin
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.28 no.4
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    • pp.152-158
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    • 2018
  • PVT (Physical Vapor Transport) method has advantages in producing high quality, large scale wafers where many researches are being carried out to commercialize nitride semiconductors. However, complex process variables cause various defects when it had non-equilibrium growth conditions. Annealing process after crystal growth has been widely used to enhance the crystallinity. It is important to set appropriate temperature, pressure, and annealing time to improve crystallinity effectively. In this study, the effect of the annealing conditions on the crystalline structure variation of the AlN single crystal grown by PVT method was investigated with synchrotron whitebeam X-ray topography, electron backscattered diffraction (EBSD), and Rietveld refinement. X-ray topography analysis showed secondary phases, sub-grains, impurities including carbon inclusion in the single crystal before annealing. EBSD analyses identified that sub-grains with slightly tilted basal plane appeared and the overall number of grains increased after the annealing process. Rietveld refinement showed that the stress caused by the temperature gradient during the annealing process between top and bottom in the hot zone not only causes distortion of grains but also changes the lattice constant.

A Study of the Structure and Luminescence Properly of BaMgAl10O17:Eu2+ Blue Phosphor using Scattering Method (Scattering법을 이용한 BaMgAl10O17:Eu2+ 청색형광체의 구조와 발광특성 연구)

  • 김광복;김용일;구경완;천희곤;조동율
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.15 no.1
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    • pp.67-74
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    • 2002
  • A phosphor for Plasma Display Panel, BaMgAl$_{10}$ O$_{17}$ :Eu$^{2+}$, showing a blue emission band at about 450nm was prepared by a solid-state reaction using BaCO$_3$, $Al_2$O$_3$, MgO, Eu$_2$O$_3$ as starting materials wish flux AlF$_3$. The study of the behaviour of Eu in BAM phosphor was carried out by the photoluminescence spectra and the Rietveld method with X-ray and neutron powder diffraction data to refine the structural parameters such as lattice constants, the valence state of Eu, the preferential site of Mg atom and the site fraction of each atom. The phenomenon of the concentration quenching was abound 2.25~2.3wt% of Eu due to a decrease in the critical distance for energy transfer of inter-atomic Eu. Through the combined Rietveld refinement, R-factor, R$_{wp}$, was 8.11%, and the occupancy of Eu and Mg was 0.0882 and 0.526 at critical concentration. The critical distance of Eu$^{2+}$ in BAM was 18.8$\AA$ at 2.25% Eu of the concentration quenching. Furthermore, c/a ratio was decreased to 3.0wt% and no more change was observed over that concentration. The maximum entropy electron density was found that the modeling of $\beta$-alumina structure in BaMgAl$_{10}$ O$_{17}$ :Eu$^{2+}$correct coincided showing Ba, Eu, O atoms of z= 1/4 mirror plane.e.ane.e.