• 제목/요약/키워드: Rietveld Method

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Lu3Al5-xGaxO12:Ce3+,Cr3+ 형광체의 결정구조 분석 및 잔광성 발광 특성 (Crystal Structure Refinement and Persistent Luminescence Properties of Lu3Al5-xGaxO12:Ce3+,Cr3+ Phosphors)

  • 김지원;김영진
    • 한국재료학회지
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    • 제30권8호
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    • pp.413-420
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    • 2020
  • Lu3Al5-xGaxO12:Ce3+,Cr3+ powders are prepared using a solid-state reaction method. To determine the crystal structure, Rietveld refinement is performed. The results indicate that Ga3+ ions preferentially occupied tetrahedral rather than octahedral sites. The lattice constant linearly increases, obeying Vegard's law, despite the strong preference of Ga3+ for the tetrahedral sites. Increasing x led to a blue-shift of the Ce3+ emission band in the green region and a change in the emission intensity. Persistent luminescence is observed from the powders prepared with x = 2-3, occurring through a trapping and detrapping process between Ce3+ and Cr3+ ions. The longest persistent luminescence is achieved for x = 2; its lifetime is at least 30 min. The findings are explained using crystal structure refinement, crystal field splitting, optical band gap, and electron trapping mechanism.

Effect of rock mineralogy on mortar expansion

  • Karaman, Kadir;Bakhytzhan, Aknur
    • Geomechanics and Engineering
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    • 제20권3호
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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).

Crystallographic Effects of Larger Indium Ion Substitution in NiFe2-xInxO4 (x = 0, 0.2, 0.5, and 1.0) System

  • Yoon, Sung-Hyun;Yoon, Chang-Sun;Kim, Byung-Ho
    • Journal of Magnetics
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    • 제10권1호
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    • pp.23-27
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    • 2005
  • The crystallographic and magnetic properties of a series of substitutions in nickel ferrite where the Fe3+ is replaced with In3+ have been investigated using X-ray diffraction (XRD) and Mössbauer spectroscopy. Information on the exact crystalline structure, lattice parameters, bond lengths and bond angles were obtained by refining their XRD profiles by a Rietveld method. All the crystal structures were found to be cubic with the space group Fd/3m. The lattice constants increased with In3+ concentration. The expansion of the tetrahedron was outstanding, indicative of the tetrahedral (A) site preference of larger indium ion. The Mossbauer spectra showed two sets of sextuplet originating from ferric ions occupying the tetrahedral sites and the octahedral (B) sites under the Neel temperature TN. Regardless of the composition x, the electric quadrupole splitting was zero within the experimental error. At x = 0.2, the magnetic hyperfine fields increased slightly, which meant that the nonmagnetic indium ions occupied preferentially the A-site. At the same time, the intensity of the B-site sub-spectra decreased markedly at the elevated temperature, indicating that the occupation of the A site by indium induced a considerable perturbation on the B site.

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

  • 김삼중;엄태형;왕웨이;서동수
    • 한국재료학회지
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    • 제18권4호
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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.

Ti-M-V 합금의 기지 및 제 2상의 수소화 특성 (Hydrogenation Characteristics of the Matrix and the Second Phases of Ti-M-V Alloys)

  • 조성욱
    • 한국수소및신에너지학회논문집
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    • 제14권2호
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    • pp.97-104
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    • 2003
  • The structural transitions of the matrix and the second phases of $Ti_{1.0}Mn_{0.9}V_{1.1}$ and $Ti_{1.0}Cr_{1.5}V_{1.7}$ alloys upon hydrogenation have been investigated at 293K. The effect of hydrogen isotope on their crystal structures has been also discussed. The crystal structures, Phase abundance and lattice parameters of the hydrides were determined by the Rietveld method using X-ray diffraction data. At the experimental temperature, the $Ti_{1.0}Mn_{0.9}V_{1.1}$ alloy and $Ti_{1.0}Cr_{1.5}V_{1.7}$ alloy revealed different structural transition processes upon hydrogenation although the crystal structures of these two alloys are both BCC at room temperature. The second phases such as Ti-rich phase with $NiTi_2$ structure and $\alpha$-Ti with HCP structure absorbed hydrogen at relatively low hydrogen pressures and the phase abundance remained almost constant. This means that it is desirable to decrease the amount of the second phases as far as possible in order to increase the effective hydrogen storage capacities of the alloys. The crystal structures of corresponding isotope hydrides, the phase abundance and the lattice parameters did not depend on the kind of hydrogen isotope, but only on the hydrogen content.

Exploration of structural, thermal and spectroscopic properties of self-activated sulfate Eu2(SO4)3 with isolated SO4 groups

  • Denisenko, Yu.G.;Aleksandrovsky, A.S.;Atuchin, V.V.;Krylov, A.S.;Molokeev, M.S.;Oreshonkov, A.S.;Shestakov, N.P.;Andreev, O.V.
    • Journal of Industrial and Engineering Chemistry
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    • 제68권
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    • pp.109-116
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    • 2018
  • $Eu_2(SO_4)_3$ was synthesized by chemical precipitation method and the crystal structure was determined by Rietveld analysis. The compound crystallizes in monoclinic space group C2/c. In the air environment, $Eu_2(SO_4)_3$ is stable up to $670^{\circ}C$. The sample of $Eu_2(SO_4)_3$ was examined by Raman, Fourier-transform infrared absorption and luminescence spectroscopy methods. The low site symmetry of $SO_4$ tetrahedra results in the appearance of the IR inactive ${\nu}_1$ mode around $1000cm^{-1}$ and ${\nu}_2$ modes below $500cm^{-1}$. The band intensities redistribution in the luminescent spectra of $Eu^{3+}$ ions is analyzed in terms of the peculiarities of its local environment.

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

  • 조한상;;류광현;유철현
    • Bulletin of the Korean Chemical Society
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    • 제21권7호
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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.

Magnetic Properties and Hyperfine Interaction of BaSrCo2(Fe1-xAlx)12O22 Hexaferrite

  • Lim, Jung Tae;Kim, Chul Sung
    • Journal of the Korean Physical Society
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    • 제73권11호
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    • pp.1679-1683
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    • 2018
  • Polycrystalline $BaSrCo_2(Fe_{1-x}Al_x)_{12}O_{22}$ (x = 0.00, 0.01, 0.05, and 0.10) samples were synthesized by polymerizable complex method. Based on the Rietveld refinement, crystal structures of the samples were found to be single-phased and determined to be rhombohedral with space group of R-3m. The hysteresis curves of the samples were measured under 15 kOe at various temperatures ranging from 4.2 and 295 K. It shows that they were not saturated with increasing Al ion contents due to the reduction of magnetic anisotropy. $M_{15kOe}$ was decreased with increasing Al ions contents. We expect that non-magnetic Al ions preferentially occupy the up-spin site of $18h_{VI}$, $3b_{VI}$, and $3a_{VI}$. The $M{\ddot{o}}ssbauer$ spectra of the samples were obtained at 295 K, and analyzed with sixsextets for Fe sites corresponding to the Y-type hexaferrite crystallography sites. The <$E_Q$> shows abrupt changes, and the <$H_{hf}$> shows abrupt decreases around x = 0.05 due to the coexistence of magnetic secondary phases.

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

  • 박일진;김철성
    • 한국자기학회지
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    • 제18권2호
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    • pp.67-70
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    • 2008
  • $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1)의 조성을 가지는 분말 시료를 sol-gel 법과 진공봉합 열처리를 이용하여 합성하였다. x선 회절기, $M\ddot{o}ssbauer$ 분광기를 이용하여 시료의 결정구조 및 Ga 이온의 점유도에 관하여 연구하였다. XRD측정결과 $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$ (x=0, 1)의 결정구조는 Ia3d의 공간그룹을 갖는 cubic 구조이며, $Tb_2Bi_1Fe_5O_{12}$$Tb_2Bi_1Ga_1Fe_4O_{12}$의 격자상수 $a_0$는 각각 $12.497\AA$, $12.465\AA$으로 분석되었다. Rietveld 분석법을 이용하여 각 이온들이 점유하는 각각의 부격자 위치를 연구하였다. $Tb_2Bi_1Ga_1Fe_4O_{12}$ 시료의 분석결과, Tb, Bi 이온은 24c 자리에, Fe 이온은 24d, 16a 자리를 점유하였으며, 비자성 이온인 Ga 이온은 모두 16a 자리를 점유하는 것으로 분석되었다. $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1)의 미시적인 자기구조를 분석하기 위해 시료들의 $M\ddot{o}ssbauer$스펙트럼을 측정하였다. 상온에서의 $M\ddot{o}ssbauer$스펙트럼 측정결과 철 이온들의 흡수 면적비는 $Tb_2Bi_1Fe_5O_{12}$의 경우 24d와 16a자리에서 각각 60.8%, 39.2%로, $Tb_2Bi_1Ga_1Fe_4O_{12}$의 경우 24d와 16a자리에서 각각 74.7%, 25.3%로 분석되었다. 철 이온들의 흡수 면적비 분석을 통해 비자성이온인 Ga은 모두 16a 자리를 점유하는 것을 알 수 있었다.

$LiATiO_4$ 스피넬 상의 결정구조 및 유전특성 (Crystal Structure and Dielectric Property of $LiATiO_4$ Spinel Phase)

  • 김정석;김남훈;천채일
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2006년도 추계학술대회 논문집 Vol.19
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    • pp.237-238
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    • 2006
  • The electrical properties such as dielectric constants and dielectric losses in the spinel samples of $LiGaTiO_4$, Li(Ga,Eu)$TiO_4$, $Li(Ga.Yb)TiO_4$ have been characterized by varying measuring temperature and frequency. The long range order structures are analyzed by rietveld refinement method. and local atomic disorder structures are analyzed by MEM (maximum entropy method). The relation between the crystal structure and dielectric properties are discussed. $LiGaTiO_4$ spinel has the IMMA with lattice constant, a = 5.86333, b=17.5872. c = 8.28375 ${\AA}$, Li-sites are partially substituted by Ga or Ti. Two crystallographic oxygen sites are partially occupied(40~50%). The dielectric constants of $LiGaTiO_4$, $LiYbTiO_4$, and $LiGa_{2/6}Eu_{1/6}Ti_{1.5}O_4$ ceramics were 127, 75 and 272, respectively at 100 kHz. The dielectric relaxation were observed in the $LiGaTiO_3$ ceramics and the temperature where dielectric loss shows maximum was $390^{\circ}C$ at 1 kHz and increased with increasing the measuring frequency.

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