• Title/Summary/Keyword: rietveld analysis

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Crystal Structure Analysis of Uranium Oxides (산화우라늄의 결정구조 분석)

  • 김정석;최용남;이창희;김시향;이영우
    • Journal of the Korean Ceramic Society
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    • v.38 no.11
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    • pp.967-972
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    • 2001
  • The crystal and defect structures of U $O_{x}$(x=2.0, 2.03, 2.14, 2.19, 2.20 and 2.26) were analysed by rietveld refinement and the results were compared to the U-O phase diagram. Neutron diffraction data were collected in the temperature range of RT~100$0^{\circ}C$. The specimens of x=2.14, 2.19, and 2.20 consisted of two phase: $UO_{2+x}$(Fm3m, a≒5.4$\AA$) and $U_4$$O_{9}$(I43d, a≒21.8$\AA$). The proportion of the $UO_{2+x}$(Fm3m) phase increased with increasing the temperature. The variation of the proportion of the two phases with temperature in the U $O_{2.2}$ and U $O_{2.18}$ samples showed some deviation from the expected values from the phase diagram especially at the high temperature range. The phase transitions ${\gamma}$longrightarrow$\beta$longrightarrow$\alpha$ of $U_4$$O_{9}$ were discussed in relation with the phase separation.eparation.ion.

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Evaluation of Hydration Characteristics and NOx-removal Performances of Cement Paste Containing Refined TiO2 Obtained from Waste Sludge (폐수 슬러지에서 정제된 TiO2를 혼입한 시멘트 페이스트의 수화특성 및 질소산화물 제거 성능 평가)

  • Yoon, Hyunno;Seo, Joonho;Kim, Seonhyeok;Bae, Jinho;Kil, Taegeon;Lee, Haeng-Ki
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.41 no.4
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    • pp.357-364
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    • 2021
  • The present study investigated the hydration properties and NOx-removal performances of the cement pastes containing three different types of TiO2. Two commercially available TiO2 (P-25 and NP-400) and refined TiO2 (GST) obtained from waste sludge were incorporated to cement paste at levels of 0, 5, 10, and 20 wt%. Isothermal calorimetry test results indicated that the TiO2 incorporation induced a notable influence on the reaction kinetics of cement paste, showing the highest cumulative heat release in the samples containing P-25, followed by NP-400 and GST. Quantitative X-ray diffractometry as calculated by the Rietveld method identified that the incorporated TiO2 promoted the formation of C-S-H, ultimately leading to the enhancement in the 28 day-compressive strength of cement pastes. As revealed by SEM/EDS analysis, the content of distributed Ti elements on the surface of the samples was in the order of P-25, GST, and NP-400. Regardless, the NOx-removal performance was the highest in the sample containing P-25, followed by NP-400 and GST.

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.

Properties of Hexaferrite Co2Y(Ba2Co2Fe12O22) Prepared by Coprecipitation Method (공침법에 의해 제조된 육방정 산화철 Co2Y(Ba2Co2Fe12O22)의 특성)

  • 신형섭;이상걸;권순주
    • Journal of the Korean Ceramic Society
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    • v.29 no.3
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    • pp.195-201
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    • 1992
  • It had been studied the structure and the magnetic properties of singel phase Co2Y(Ba2Co2Fe12O22) powder, one of the hexagonal ferrite. The material was successfully prepared by a commercially applicable coprecipitation method. Adding asqueous solution of BaCl2, CoCl2 and FeCl2(Ba2+:Co2+:Fe2+=1:1:6 in mole ratio) to a mixture of NaOH and hydrogen peroxide solution, coprecipitate was formed with rapid oxidation of ferrous to ferric ion. The coprecipitate transformed to single phase Co2Y powder at heat treatment temperatures as low as 900$^{\circ}C$. The shape of Co2Y particles obtained at 900$^{\circ}C$ was hexagonal plate-like (diameter∼$\mu\textrm{m}$, aspect ratio>10). The structure of the Co2Y was refined by a Rietveld analysis of the measured X-ray diffractogram. The lattice parameters are ao=5.8602${\AA}$ and co=43.512${\AA}$. Co2Y is a soft magnetic material with saturation magnetization 30 emu/g and coecivity 170 . A standard X-ray diffraction pattern for Co2Y is proposed as well.

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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.

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).

Synthesis of Iron Oxide Using Ferrous Sulfate and Ammonia Water (황산제일철과 암모니아수를 이용한 산화철 합성)

  • Kim, Sam-Joong;Eom, Tae-Hyoung;Wang, Wei;Suhr, Dong-Soo
    • Korean Journal of Materials Research
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    • v.18 no.4
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    • pp.218-221
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    • 2008
  • A $Fe(OH)_2$ suspension was prepared by mixing iron sulfate and a weak alkali ammonia solution. Following this, iron oxides were synthesized by passing pure oxygen through the suspension (oxidation). The effects of different reaction temperatures ($30^{\circ}C$, $50^{\circ}C$, $70^{\circ}C$) and equivalent ratios ($0.1{\sim}10.0$) on the formation of iron oxides were investigated. An equilibrium phase diagram was established by quantitative phase analysis of the iron oxides using the Rietveld method. The equilibrium phase diagram showed a large difference from the equilibrium phase diagram of Kiyama when the equivalent ratio was above 1, and single $Fe_3O_4$ phase only formed above an equivalent ratio 2 at all reaction temperatures. Kiyama synthesized iron oxide using iron sulfate and a strong alkali NaOH solution.

Hydrogen Storage Properties of Hydriding-Dehydriding Cycled Magnesium-Nickel-Iron Oxide Alloy

  • Song, Myoung Youp;Kwon, Sung Nam;Park, Hye Ryoung;Kim, Byoung-Goan
    • Korean Journal of Metals and Materials
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    • v.50 no.2
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    • pp.171-175
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    • 2012
  • By measuring the absorbed hydrogen quantity as a function of the number of cycles, the cycling properties of the Mg-15 wt%Ni-5 wt%$Fe_2O_3$ alloy were investigated. The absorbed hydrogen quantity decreased as the number of cycles increased. The $H_a$ value varied almost linearly with the number of cycles. The maintainability of absorbed hydrogen quantity at n=100 was 89.0% for the hydriding reaction time of 10 min. After the $150^{th}$ hydriding-dehydriding cycle, Mg, $Mg_2Ni$, $Mg(OH)_2$, MgO, and Fe were observed. The phases were analyzed by Rietveld analysis from the XRD patterns of the Mg-15 wt%Ni-5 wt%$Fe_2O_3$ alloy after 150 hydriding-dehydriding cycles. The crystallite size and strain of Mg were then estimated with the Williamson-Hall technique.

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.

Mössbauer Study of Tb2Bi1GaxFe5-xO12(x=0, 1) (Tb2Bi1GaxFe5-xO12(x=0, 1)의 뫼스바우어 분광연구)

  • Park, Il-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.18 no.2
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    • pp.67-70
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    • 2008
  • $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) fabricated by sol-gel and vacuum sealed annealing process. $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) have been studied by x-ray diffraction(XRD), vibrating sample magnetometer, and $M\ddot{o}ssbauer$ spectroscopy. The crystal structures were found to be a cubic garnet structure with space group Ia3d. The determined lattice constants $a_0$ of x = 0, and 1 are $12.497\AA$, and $12.465\AA$, respectively. The distribution of gallium and iron in $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$ is studied by Rietveld refinement. Based on Rietveld refinement results, the terbium and bismuth ions occupy the 24c site, iron ions occupy the 24d, l6a site, and nonmagmetic gallium ions occupy the 16a site. In order to verify the magnetic site occupancy of iron and gallium, we have taken $M\ddot{o}ssbauer$ spectra for $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) at room temperature. From the results of $M\ddot{o}ssbauer$ spectra analysis, the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 60.8 % and 39.2 %, respectively, and the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 74.7 % and 25.3 %, respectively. It is noticeable that all of the nonmagnetic Ga atoms occupy the 16a site by vacuum annealing process.