• Title/Summary/Keyword: Rietveld Analysis

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A Study of Mineral Quantification on Clay-Rich Rocks (점토질 암석의 광물정량 분석법 연구)

  • Byeong-Kook, Son;Gi-O, An
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.4
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    • pp.431-445
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    • 2022
  • A quantitative phase analysis method of X-ray powder diffraction was studied to determine the mineral content of clay-rich rocks practically as well as effectively. For quantitative X-ray powder diffraction analysis of the clay-rich rocks, it is necessary to prepare whole-rock powder samples with a random orientation by side mounting method. In addition, for the identification of the clay minerals in the rock, it is required to prepare an oriented mount specimen with a clay particle size of 2 ㎛ or less, ethylene glycol treatment, and heat treatment. RIR (reference intensity ratio) and Rietveld method were used for the quantitative analysis of the clay-rich rocks. It was possible to obtain the total clay and the non-clay minerals contents from the whole-rock X-ray diffraction profiles using the RIR values. In addition, it was possible to calculate the relative content of each clay mineral from the oriented X-ray diffraction profiles of the clay particle size and assign it to the total clay. In the Rietveld method of whole-rock X-ray diffraction, effective quantitative values were obtained from the Rietveld diffraction patterns excluded the region of less than 10 degrees (2θ). Similar quantitative values were shown in not only the RIR but the Rietveld methods. Therefore, the analysis results indicate a possibility of a routine quantitative analysis of clay-rich rocks in the laboratory. However, quantitative analysis of clay minerals is still a challenge because there are numerous varieties of clay minerals with different chemical and structural characteristics.

Microscopic Characterization of Cement Composites with Carbon Nanotubes (탄소나노튜브가 첨가된 시멘트복합체의 미시적특성분석)

  • Kim, Young-Min;Lee, Gun Cheol
    • Proceedings of the Korean Institute of Building Construction Conference
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    • 2019.11a
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    • pp.176-177
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    • 2019
  • As a result of the Rietveld analysis to determine the effect of carbon nanotubes on the hydration products of cement composites, the quantitative difference of hydration products according to the addition rate of carbon nanotubes was not significant. Ettringite, an early hydration product, was measured to be slightly higher than the planes with carbon nanotubes over all ages. Therefore, it seems that carbon nanotubes have no effect on the hydration production in cement paste.

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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.

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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Synthesis of $LiCoO_{2}$ powders from precursors prepared by precipitation process

  • Park, Cheong-Song;La, Jung-In;Kim, Do-Youn
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.12 no.2
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    • pp.87-90
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    • 2002
  • $LiCoO_{2}$ powders were synthesized at various temperatures using lithium hydroxide and cobalt hydroxide as precursors prepared by precipitation process and freeze-drying. In this study, the$LiCoO_{2}$ samples were synthesized via a solid state reaction with various LiOH concentration between 10 % and 30 % excess. And $LiCoO_{2}$powders were calcined at 600~$800^{\circ}C$ in a short time. Measurements of XRD and SEM were performed to characterize the properties of the prepared materials. The effect of amount of Li ions on the structural change in powder has been examined using the XRD analysis. For the not added excess of LiOH, CoOOH phase presented in the XRD pattern of $LiCoO_{2}$ due to loss of Li ions during firing. The morphology and particle size of the powders were examined using SEM. The obtained powders are high temperature-$LiCoO_{2}$HT-LiCoO$_{2}$) and homogeneous with the range of grain size in the order of hundreds of nanometers. The effects of variation of LiOH concentration on the structural change in powder were investigated using the Rietveld analysis. As an analysis result, c/a is constant by 4.99 on all occasions. Finally, the structure of HT-$LiCoO_{2}$ was simulated by the commercial software $Creius^{2}$(Molecular Simulations, Inc.) from the results of Rietveld analysis.

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.

Rietveld Analysis of YBCO superconductor (YBCO 고온 초전도체의 Rietveld 해석 연구)

  • ;;;Fan Zhangguo
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 1995.05a
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    • pp.182-186
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    • 1995
  • In this pacer, it is examined and confirmed that the R factor which is compensated after analyzing the characteristics of superconductor resulted from this experimented theory with the computer simulation, is refined to R$\sub$WP/=8.83[%], R$\sub$P/=6.47[%], R$\sub$I/=10.08[%], RF=7.19[%], R/eub E/=3.76(%), and on the basis of these experimental data, the significant parameter such as the scale factor(s) and the zero point shift(Z) and FWHM value(U,V,W) are optimized as follows; S =72.0827E-3, Z=0.2146, U=4.2761E-2, V=1.7983E-2, and W=2.6768E-2

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Synchrotron X-ray Powder Diffraction Study of CFC-13 Loaded Zeolite LSX (제올라이트 LSX에서의 CFC-13 분자체 흡착에 관한 결정학적 연구)

  • Lee, Yong-Jae;Lee, Jong-Won;Yoon, Ji-Ho
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.3
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    • pp.307-312
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    • 2008
  • Rietveld analysis using synchrotron X-ray powder diffraction data collected at 15 K reveals that CFC-13 ($CF_{3}Cl;$ chlorotrifluoromethane) sorbed on Na,K-LSX binds through fluorine to sodium ions around the single 6-ring aperture in the supcrgage.