• Title/Summary/Keyword: XRD-Rietveld analysis

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Effects of Crystallization Behavior on Microwave Dielectric Properties of CaMgSi2O6 Glass-Ceramics

  • Choi, Bo Kyeong;Kim, Eung Soo
    • Journal of the Korean Ceramic Society
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    • v.50 no.1
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    • pp.70-74
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    • 2013
  • Dependence of microwave dielectric properties on the crystallization behaviors of $CaMgSi_2O_6$ (diopside) glass-ceramics was investigated with different heat treatment methods (one and/or two-step). The crystallization behaviors of the specimens, crystallite size and degree of crystallization, were evaluated by differential thermal analysis (DTA), scanning electron microscope (SEM) and X-ray diffraction (XRD) analysis by combined Rietveld and reference intensity ratio (RIR) methods. With an increase in heattreatment temperature, the dielectric constant (K) and the quality factor (Qf) increased due to the increase of the crystallite size and degree of crystallization. The specimens heat-treated by the two-step method had a higher degree of crystallization than the specimens heat-treated by the one-step method, which induced improvement in the quality factor (Qf) of the specimens.

Magnetic Properties of Sn1-xFexO2 Thin Films and Powders Grown by Chemical Solution Method

  • Li, Yong-Hui;Shim, In-Bo;Kim, Chul-Sung
    • Journal of Magnetics
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    • v.14 no.4
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    • pp.161-164
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    • 2009
  • Iron-doped $Sn_{1-x}Fe_xO_2$ (x = 0.0, 0.05, 0.1, 0.2, 0.33) thin films on Si(100) substrates and powders were prepared by a chemical solution process. The x-ray diffraction (XRD) patterns of the $Sn_{1-x}Fe_xO_2$ thin films and powders showed a polycrystalline rutile tetragonal structure. Thermo gravimetric (TG) - differential thermal analysis (DTA) showed the final weight loss above $430{^{\circ}C}$ for all powder samples. According to XRD Rietveld refinement of the powders, the lattice parameters and unit cell volume decreased with increasing Fe content. The magnetic properties were characterized using a vibrating sample magnetometer (VSM) and M$\ddot{o}$ssbauer spectroscopy. The thin film samples with x = 0.1 and 0.2 showed paramagnetic properties but thin films with x = 0.33 exhibited ferromagnetic properties at room temperature. Mossbauer studies revealed the $Fe^{3+}$ valence state in the samples. The ferromagnetism in the samples can be interpreted in terms of the direct ferromagnetic coupling of ferric ions via an electron trapped in a bridging oxygen deficiency, which can be explained using the F-center exchange model.

Structural Characterization of the (TEX)$Sr_2Co_0.5Nb(Ta)_0.5O_4$(/TEX) and (TEX)$Sr_3CoNb(Ta)O_7$(/TEX)

  • Jo, Han Sang;Ri-Zhu Yin;Ryu, Gwang Hyeon;Yu, Cheol Hyeon
    • Bulletin of the Korean Chemical Society
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    • v.21 no.7
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    • pp.679-684
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    • 2000
  • The Sr2Co0.5Nb(Ta)0.5O4 and Sr3CoNb(Ta)O7 compounds, both with Ruddlesden-Popper structures, have been synthesized by the ceramic method at $1150^{\circ}C$ under atmospheric pressure. The crystallographic structure of the compounds was assigned to the tetr agonal system with space group 14/mmm by X-ray diffraction(XRD) Rietveld refinement. The reduced lattice volume and lattice parameters increased as the Ta with 5d substitutes for the Nb with 4d in the compounds. The Co/Nb(Ta)O bond length has been determined by X-ray absorption spectroscopic(EXAFS/XANES) analysis and the XRD refinement. The CoO6,octahedra were tetragonally distorted by elongation of Co-O bond along the c-axis. The magnetic measurement shows the compounds Sr2Co0.5Nb(Ta)0.5O4 and Sr3CoNb(Ta)O7 have paramagnetic properties and the Co ions with intermediate spin sates between high and low spins in D4h symmetry. All the compounds showed semiconducting behavior whose electrical conductivity increased with temperature up to 1000 K. The electrical conductiviy increased and the activation energy for the conduction decreased as the number of perovskite layers increased in the compounds with chemical formula An+1BnO3n+1.

Mineral Compositions of Korean Dancheong Pigment Products using Quantitative XRD (정량 X-선 회절분석을 이용한 국내시판 단청안료의 광물조성 연구)

  • Moon, Dong Hyeok;Han, Min Su;Jeong, Hye Young;Go, In Hee;Cho, Hyen Goo
    • Journal of Conservation Science
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    • v.32 no.3
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    • pp.403-416
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    • 2016
  • Mineral composition and content of 22 Korean Dancheong pigment products were obtained by Rietveld quantitative analysis. Jubosa, Hwang, Seokrok, Seokcheong and Hobun consist of pure cinnabar, orpiment, malachite, azurite and calcite (or aragonite), respectively. Whereas Seokganju, Hwangto, Noerok, Lapis lazuli, Baekto and Cockie hobun mainly consist of hematite, goethite, celadonite, lazurite, kaolin mineral and portlandite, respectively. And they all consist of soil minerals (quartz, feldspar, sericite and vermiculite) and filler minerals in the industry field (calcite, gypsum and anhydrite) at a different content. Quantitative XRD proved more useful method to determined exact mineral composition and content than chemical or microscopical data. If this method utilize for specification of natural pigment product, it is considered to be applicable in restoration technology and conservation science field.

USE OF NEAR INFRARED FOR THE QUANTITATIVE ANALYSES OF BAUXITE

  • Walker, Graham S.;Cirulis, Robyn;Fletcher, Benjimin;Chandrashekar, S.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1171-1171
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    • 2001
  • Quantitative analysis is an important requirement in exploration, mining and processing of minerals. There is an increasing need for the use of quantitative mineralogical data to assist with bore hole logging, deposit delineation, grade control, feed to processing plants and monitoring of solid process residues. Quantitative analysis using X-Ray Powder Diffraction (XRD) requires fine grinding and the addition of a reference material, or the application of Rietveld analysis to XRD patterns to provide accurate analysis of the suite of minerals present. Whilst accurate quantitative data can be obtained in this manner, the method is time consuming and limited to the laboratory. Mid infrared when combined with multivariant analysis has also been used for quantitative analysis. However, factors such as the absorption coefficients and refractive index of the minerals requires special sample preparation and dilution in a dispersive medium, such as KBr to minimize distortion of spectral features. In contrast, the lower intensity of the overtones and combinations of the fundamental vibrations in the near infrared allow direct measurement of virtually any solid without special sample preparation or dilution. Thus Near Infrared Spectroscopy (NIR) has found application for quantitative on-line/in line analysis and control in a range of processing applications which include, moisture control in clay and textile processing, fermentation processes, wheat analysis, gasoline analysis and chemicals and polymers. It is developing rapidly in the mineral exploration industry and has been underpinned by the development of portable NIR spectrometers and spectral libraries of a wide range of minerals. For example, iron ores have been identified and characterized in terms of the individual mineral components using field spectrometers. Data acquisition time of NIR field instruments is of the order of seconds and sample preparation is minimal. Consequently these types of spectrometers have great potential for in-line or on-line application in the minerals industry. To demonstrate the applicability of NIR field spectroscopy for quantitative analysis of minerals, a specific example on the quantification of lateritic bauxites will be presented. It has been shown that the application of Partial Least Squares regression analysis (PLS) to the NIR spectra can be used to quantify chemistry and mineralogy in a range of lateritic bauxites. Important, issues such as sampling, precision, repeatability, and replication which influence the results will be discussed.

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Structure Refinement and Equation of State Studies of the Exsoluted Ilmenite-Hematite (티탄철석-적철석 용출시료의 구조분석과 상태방정식 연구)

  • Hwang, Gil-Chan;Kim, Young-Ho
    • Journal of the Mineralogical Society of Korea
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    • v.24 no.3
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    • pp.195-204
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    • 2011
  • Exsolution intergrowth of ilmenite and hematite was studied by the Rietveld refinement method. According to the analysis on these two structural analog minerals, it was found that octahedron (M2) of Ti in ilmenite is in the least deformation, then that (M1) of Fe in ilmenite is deformed next, and octaheron deformation of Fe in hematite is between M1 and M2. High pressure compression experiment was performed up to 5.8 GPa, where two minerals' XRD peaks merged completely. Ilmenite shows normal compression behavior, whereas hematite shrinks in very small amount. This kind of abnormal behavior might be due to the differential response to the applied pressure corresponding to the different compressibilities of the minerals each other.

Phase evaluation of Fe/Co pigments coated porcelain by rietveld refinement (리트벨트 정밀화법에 의한 Fe/Co 안료가 코팅된 도자기의 상분석)

  • Nam-Heun Kim;Kyung-Nam Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.33 no.5
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    • pp.174-180
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    • 2023
  • Porcelain (white ware, celadon ware) coated with a ferrous sulfate and ferrous/cobalt sulfate was sintered at 1250℃. The specimens were investigated by HR-XRD, FE-SEM, HR-EDS, and UV-vis spectrophotometer. Through X-ray rietveld quantitative analysis, quartz and mullite were found to be the main phases for white ware, and mullite and plagioclase were found to be the main phases for celadon ware. When the pigment of ferrous/cobalt sulfate was applied, were identified as an andradite phase for celadon ware and a spinel phase for the white ware, and the amorphous phase, respectively. The L* value, which was the brightness of the specimen, was 72.01, 60.92 for white ware and celadon ware, respectively. The ferrous and ferrous/cobalt pigment coated porcelain had L* values of 44.89, 52.27 for white ware and celadon ware, respectively; with a* values of 2.12, 1.40, an d at b* values of 1.45 and 13.79. As for the color of the specimens, it was found that the L* value was greatly affected by the white ware, and the b* value differed greatly depending on the clay. It was thought to be closely related to the production of the secondary phase such as Fe2O3 and andradite phase produced in the surface layer.

Thermal Properties of 0.9CaMgSi2O6-0.1MgSiO3 Glass-Ceramics

  • Jeon, Chang-Jun;Sun, Gui-Nam;Lee, Jong-Kyu;Ju, Han-Sae;Kim, Eung-Soo
    • Journal of the Korean Ceramic Society
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    • v.49 no.1
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    • pp.111-117
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    • 2012
  • Dependencies of thermal properties on the crystallization behavior of $0.9CaMgSi_2O_6-0.1MgSiO_3$ glass-ceramics were investigated as a function of heat-treatment temperature from $750^{\circ}C$ to $950^{\circ}C$. The crystallization behavior of the specimens depended on the heat-treatment temperature, which could be evaluated by differential thermal analysis (DTA), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction (XRD) analysis by the Rietveld-reference intensity ratio (RIR) combined procedure. With an increase of the heat-treatment temperature, the thermal conductivity and thermal diffusivity of the heat-treated specimens increased. These results could be attributed to the increase of crystallization with heat-treatment temperature. However, the specific heat capacity of the heat-treated specimens was not affected by the heat-treatment temperature. The thermal conductivities measured from $25^{\circ}C$ to $100^{\circ}C$ were also discussed for application to lighting-emitting diode (LED) packages and substrate materials.

Reinvestigation of Dion-Jacobson Phases CsCa2Nb2MO9 (M = Fe and Al)

  • Hong, Young-Sik
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.853-856
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    • 2006
  • Dion-Jacobson phases $CsCa_2Nb_2FeO_9$ and $CsCa_2Nb_2AlO_9$ were reinvestigated by the Rietveld analysis of powder X-ray diffraction (XRD) method, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). These nominal compounds, previously known as the oxygen-deficient layered perovskites with the sequences of $NbO_6-MO_4-NbO_6$ in tripled slab, in fact, were mixed phases of n = 3 Dion-Jacobson phases and impurities such as $Ca_2NbFeO_6$ and $Ca_3Al_2O_6$. The difference of morphology and chemical in-homogeneity between Dion-Jacobson phases and impurities could be clearly identified by scanning electron microscopy with energy-dispersive X-ray spectroscopy. The chemical composition of $CsCa_2Nb_2FeO_9$ was calculated into $Cs_{0.59}Ca_{2.64}Nb_{2.92}Fe_{0.81}$ in small agglomerate crystals and $Cs_{0.95}Ca_{1.97}Nb_{3.08}Fe_{0.15}$ in long plate-like crystals.

Effect of rock mineralogy on mortar expansion

  • Karaman, Kadir;Bakhytzhan, Aknur
    • Geomechanics and Engineering
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    • v.20 no.3
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    • pp.233-241
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    • 2020
  • Alkali-silica reaction (ASR) is among one of the most important damaging mechanisms in concrete, depending primarily on aggregates which contain reactive minerals. However, expansion in concrete may not directly relate to the reactive minerals. This study aims to investigate the influence of ASR and the expansion of mortar bars depending on aggregate type containing various components such as quartz, clay minerals (montmorillonite and kaolinite) and micas (muscovite and biotite). In this study, the accelerated mortar bar tests (AMBT) were performed in two conditions (mortar bars in the same and sole NaOH solutions). Petrographic thin section studies, X-ray diffraction (XRD) analysis (Rietveld method), scanning electron microscopy (SEM) and chemical analyses were carried out. This study showed that quartzite bars led to increase in expansion values of mortar bars in diabase-1 and andesite when these were in the same NaOH solution. However, three samples (basalt, quartzite and claystone) were found having ASR expansion based on the AMBT when the special molds were used for each sample. SEM study revealed that samples which exhibit highest expansions according to AMBT had a generally rough surface and acicular microstructures in or around the micro-cracks. Basalt and quartzite showed more variable in major oxides than those of other samples based on the chemical analyses, SEM studies and AMBT. This study revealed that the highest expansions were observed to source not only from reactive aggregates but also from alteration products (silicification, chloritization, sericitization and argillisation), phyllosilicates (muscovite, biotite and vermiculite) and clays (montmorillonite and kaolinite).