• Title/Summary/Keyword: rietveld analysis

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Layered Metal Hydroxides Containing Calcium and Their Structural Analysis

  • Kim, Tae-Hyun;Heo, Il;Paek, Seung-Min;Park, Chung-Berm;Choi, Ae-Jin;Lee, Sung-Han;Choy, Jin-Ho;Oh, Jae-Min
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1845-1850
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    • 2012
  • Layered metal hydroxides (LMHs) containing calcium were synthesized by coprecipitation in solution having two different trivalent metal ions, iron and aluminum. Two mixed metal solutions ($Ca^{2+}/Al^{3+}$ and $Ca^{2+}/Fe^{3+}$ = 2/1) were added to sodium hydroxide solution and the final pH was adjusted to ~11.5 and ~13 for CaAl-and CaFe-LMHs. Powder X-ray diffraction (XRD) for the two LMH samples showed well developed ($00l$) diffractions indicating 2-dimensional crystal structure of the synthesized LMHs. Rietveld refinement of the X-ray diffraction pattern, the local structure analysis through X-ray absorption spectroscopy, and thermal analysis also confirmed that the synthesized precipitates show typical structure of LMHs. The chemical formulae, $Ca_{2.04}Al_1(OH)_6(NO_3){\cdot}5.25H_2O$ and $Ca_{2.01}Fe_1(OH)_6(NO_3){\cdot}4.75H_2O$ were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Particle morphology and thermal behavior for the synthesized LMHs were examined by field emission scanning electron microscopy and thermogravimetricdifferential scanning calorimetry.

A $M\"{o}ssbauer$ Spectroscopic Sthdy of Ion Distribution in $Ba_{2}{(Co,Zn)}_{2}Fe_{12}O_{22}$ ($M\"{o}ssbauer$ 분광 분석에 의한 $Ba_{2}{(Co,Zn)}_{2}Fe_{12}O_{22}$ 내의 이온 분포 연구)

  • 최상준;권순주
    • Journal of the Korean Magnetics Society
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    • v.6 no.2
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    • pp.73-79
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    • 1996
  • Y-type hexagonal ferrites$(Ba_{2}Me_{2}Fe_{12}O_{22}:Me=transition metal)$ have promising electromagnetic properties in GHz range. Co and Zn are good candidates for the transition metal. To understand their role on the properties, it is thus necessary to study the ion(s) distribution in that complex Y-type hexagonal ferrite structure. The authors report Mossbauer spectroscopic results from very reliable samples, which has been extensively characterized by chemical analysis, Rietveld analysis of X-ray diffraction patterns, and magnetic property measurements. Analyzing two samples, $Co_{2}Y$ and $Co_{1.6}Zn_{0.4}Y$, conclusions are made as follow: (1) Co ions prefer the tetrahedral interstitial sites in the S-block $(6c_{IV})$ and the octahedral sites $(18h_{VI})$ at the interface of S- and T-block. (2) Partial substitution of Co with Zn (within the experimental range) does not disturb the Fe distribution.

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Magnetocaloric Properties of AlFe2B2 Including Paramagnetic Impurities of Al13Fe4

  • Lee, J.W.;Song, M.S.;Cho, K.K.;Cho, B.K.;Nam, Chunghee
    • Journal of the Korean Physical Society
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    • v.73 no.10
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    • pp.1555-1560
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    • 2018
  • $AlFe_2B_2$ produced by using a conventional arc melter has a ferromagnetic material with a Curie temperature ($T_C$) of around 300 K, but the arc-melt generates paramagnetic $Al_{13}Fe_4$ impurities during the synthesis of $AlFe_2B_2$. Impurities are brought to cause a decrease in magnetocaloric effects (MCEs). To investigate the effects of $Al_{13}Fe_4$ impurities on MCEs, we prepared and compared ascast and acid-treated samples, where the acid treatment was performed to remove the $Al_{13}Fe_4$ impurities. For the structural analysis, powder X-ray diffraction was carried out, and the measured data were subjected to a Rietveld refinement. The presence of $Al_{13}Fe_4$ impurities in the as-cast sample was observed in the phase analysis measurements. Magnetic properties were investigated by using Superconducting Quantum Interference Device (SQUID) measurements for the as-cast and the acid-treated $AlFe_2B_2$ samples. From isothermal magnetization measurements, Arrott plots were obtained showing that the transition of $AlFe_2B_2$ has a second-order magnetic phase transition (SOMT). The $T_C$ and the saturation magnetization increased for the acid-treated sample due to removal of the paramagnetic impurities. As a consequence, the magnetic entropy change ($-{\Delta}S$) increased in the pure $AlFe_2B_2$ samples, but the full width at half maximum in the plot of $-{\Delta}S$ vs. T decreased due to the absence of impurities.

Preparation and characterization of new perovskite compounds $(Na_{0.5}Sr_{0.5})(M_{0.5}N_{0.5})O_3$(MTi,Zr N=Ta,Nb)

  • Chung, Hoon-Taek;Tetsuro Nakamura;Mitsuru Itoh
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1997.06a
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    • pp.49-51
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    • 1997
  • New complex perovskite compounds (Na0.5Sr0.5)(Ti0.5Nb0.5)O3, (Na0.5Sr0.5)(Zr0.5Ti0.5)O3 and (Na0.5Sr0.5)(Ti0.5Ta0.5)O3 have been prepared. The crystal structures of these compounds were determined by powder X-ray Rietveld analysis. The crystal structure of (Na0.5Sr0.5)(Ti0.5Nb0.5)O3 and (Na0.5Sr0.5)(Zr0.5Ta0.5)O3 was Pmmn, and that of (Na0.5Sr0.5)(Ti0.5Nb0.5)O3 was I4/mmm. All these compounds showed the superstructure due to the oxygen octahedron distortion. The selected bond distances and bond angles were calculated by the OFFER. The octahedron distortion for each sample, which was measured from the bond distances and bond angles, showed the following order: (Na0.5Sr0.5)(Z0.5Ta0.5)O3> (Na0.5Sr0.5)(Ti0.5Nb0.5)O3 > (Na0.5Sr0.5)(Ti0.5Ta0.5)O3. Dielectric properties were measured for the samples. In this study, the crystal structure and dielectric properties of the new complex perovskite structures and discussed.

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Crystal Structures, Electrical Conductivities and Electrochemical Properties of LiCo1-XMgxO2(x=0.03) for Secondary Lithium Ion Batteries (리튬 2차 전지용 LiCo1-XMgxO2(x=0.03)의 결정구조, 전기전도도 및 전기화학적 특성)

  • Kim, Ho-Jin;Chung, Uoo-Chang;Jeong, Yeon-Uk;Lee, Joon-Hyung;Kim, Jeong-Joo
    • Journal of the Korean Ceramic Society
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    • v.42 no.9 s.280
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    • pp.602-606
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    • 2005
  • [ $LiCoO_{2}$ ] is the most common cathode electrode materials in Lithium-ion batteries. $LiCo_{0.97}Mg_{0.03}O_2$ was synthesized by the solid-state reaction method. We investigated crystal structures, electrical conductivities and electrochemical properties. The crystal structure of $LiCo_{0.97}Mg_{0.03}O_2$ was analyzed by X-ray powder diffraction and Rietveld refinement. The material showed a single phase of a layered structure with the space group R-3m. The lattice parameter(a, c) of $LiCo_{0.97}Mg_{0.03}O_2$ was larger than that of $LiCoO_2$. The electrical conductivity of sintered samples was measured by the Van der Pauw method. The electrical conductivities of $LiCoO_2$ and $LiCo_{0.97}Mg_{0.03}O_2$ were $2.11{\times}10^{-4}\;S/cm$ and $2.41{\times}10^{-1}\;S/cm$ at room temperature, respectively. On the basis of the Hall effect analysis, the increase in electrical conductivities of $LiCo_{0.97}Mg_{0.03}O_2$ is believed due to the increased carrier concentrations, while the carrier mobility was almost invariant. The electrochemical performance was investigated by coin cell test. $LiCo_{0.97}Mg_{0.03}O_2$ showed improved cycling performance as compared with $LiCoO_2$.

Structures and Electrochemical Properties of LiNi0.5-xCo2x}Mn0.5-xO2 as Cathode Materials for Lithium-ion Batteries

  • Choi, Hyun-Chul;Kim, Ho-Jin;Jeong, Yeon-Uk;Jeong, Soo-Hwan;Cheong, In-Woo;Jung, Uoo-Chang
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2603-2607
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    • 2009
  • $LiNi_{0.5-x}Co_{2x}Mn_{0.5-x}O_{2}$ (x = 0, 0.1, 1/6, 1.2, 0.3) were synthesized by the solid-state reaction method. The crystal structure was analyzed by X-ray powder diffraction and Rietveld refinement. $LiNi_{0.5-x}Co_{2x}Mn_{0.5-x}O_{2}$ samples give single phases of hexagonal layered structures with a space group of R-3m for x = 0.1, 1/6, 0.2, and 0.3. The lattice constants of a and c-axis were decreased with the increase in Co contents in samples. The thickness of MO2 slab was decreased and inter-slab distance was increased with the increase in Co contents in $LiNi_{0.5-x}Co_{2x}Mn_{0.5-x}O_{2}$. According to XPS analysis, the valence states of Mn, Co, and Ni in the sample are mainly +4, +3, and +3, respectively. The discharge capacity of 202 mAh/g at 0.1C-rate in the potential range of 4.7 - 3.0 V was obtained in $LiNi_{0.3}Co_{0.4}Mn_{0.3}O_2$ sample, and $LiNi_{0.4}Co_{0.2}Mn_{0.4}O_2$ gives excellent cycle performance in the same potential range.

The Study on Phase Transition Pressure of Donor doped Pb(Zr0.52Ti0.48)O3 Ceramics with Diamond Anvil Cell (다이아몬드 엔빌 셀을 이용한 Donor doped Pb(Zr0.52Ti0.48)O3 세라믹스의 상전이 압력 연구)

  • Cho, Kyung-Ho;Ko, Young-Ho;Seo, Chang-Eui;Kim, Kwang-Joo
    • Journal of the Korean Ceramic Society
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    • v.48 no.5
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    • pp.471-478
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    • 2011
  • Investigations of crystal structure and phase transition of $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics doped with A-site substitution impurity (La, Nd) or B-site substitution impurity (Sb, Nb) at 2 mol% concentration were carried out. X-ray diffraction patterns of impurities doped $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics have been measured at pressures up to ~5 GPa with diamond anvil cell and synchrotron radiation. The patterns were obtained at room temperature using methanol-ethanol mixture as pressure-transmitting media. In order to refine the crystal structure, Rietveld analysis has been performed. The structures of impurities doped $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics are tetragonal in space group P4mm at ambient pressure and are transformed into a cubic phase in space group Pm$\bar{3}$m as the pressure increases. In this study, when A-site substitution donor $La^{3+}$ or $Nd^{3+}$ ion was added to $Pb(Zr_{0.52}Ti_{0.48})O_3$ ceramics, the phase transition phenomena showed up at the pressure of 2.5~4.6 GPa, but when B-site substitution donor $Nb^{5+}$ or $Sb^{5+}$ ion was added to it, the phase transition appeared at relatively lower pressure of 1.7~2.6 GPa.

Physical and Chemical Properties of Cement Mortar with Gamma-C2S

  • Lee, Sung-Hyun;Kim, Kyungnam;Mabudo, Mabudo;Song, Myong-Shin
    • Journal of the Korean Ceramic Society
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    • v.53 no.2
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    • pp.194-199
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    • 2016
  • Presently, for the cement industry, studies that seek to reduce $CO_2$, because of the development of the plastic industry and demand for reduction of energy use, have been actively conducted among them, studies attempting to use Gamma-$C_2S({\gamma}-C_2S)$ to fix $CO_2$ have been actively conducted. The ${\gamma}-C_2S$ compound has an important function in reacting to $CO_2$ and stiffening through carbonatization in the air. The ${\gamma}-C_2S$ compound, reacting to $CO_2$ in the air, generates $CaCO_2$ within the pore structure of cement materials and densifies the pore structure this leads to an improvement of the durability and to the characteristic of resistance against neutralization. Therefore, in this experiment, in order to synthesize ${\gamma}-C_2S$, limestone sludge and waste foundry sands are used these materials are plasticized for 30 or 60 minutes at $1450^{\circ}C$, and are prevented from being cooled in the temperature range of $30{\sim}1000^{\circ}C$ when they are about to be cooled. XRD analysis and XRF analysis are used to determine the effects of this process on ${\gamma}-C_2S$ synthesization, the temperature at which a thing is plasticized, and the conditions for cooling that obtain in the plasticized clinker also, in order to confirm the $CO_2$ capture function, analysis of the major hydration products is conducted through an analysis of carbonatization depth and compressive strength, and through MIP analysis and XRD Rietveld analysis. As a result of these analyses, it is found that when ${\gamma}-C_2S$ was synthesized, the clinker that was plasticized at $1450^{\circ}C$ for one hour demonstrated the highest yield rate the sample with which the ${\gamma}-C_2S$ was mixed generated $CaCO_3$ when it reacted with $CO_2$ therefore, carbonatization depth and porosity were reduced, and the compressive strength was increased.

Crystal structure refinement and microwave dielectric characteristic of $(1-x)CaTiO_3-x(La_{1/3}Nd_{1/3})TiO_3$ ($(1-x)CaTiO_3-x(La_{1/3}Nd_{1/3})TiO_3$계의 결정구조 해석 및 마이크로파 유전 특성)

  • 조남웅;성경필;문종하;최주현
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.3
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    • pp.478-486
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    • 1998
  • $CaTiO_3-x(La_{1/3}Nd_{1/3}TiO_3\;(0\le \textrm x\le0.8)$ system was prepared by reaction of $CaCO_3,\;LaO_3,\;Nd_2CO_3$ and ,TEX>$TiO_2$ mixture at 1673 K, which can be applied for microwave dielectric ceramic materials. The lattice parameters of(1-x))$CaTiO_3-x(La_{1/3}Nd_{1/3}TiO_3\;(0\le \textrm x\le0.8)$ system increased with the increase of x. Its structure was investigated by Rietveld profile-analysis of XRD in detail. Cations $ La^{3+}$ and Nd^{3+}$ were located at the $Ca^{2+}$ site in the range of $0\le \textrm x\le0.8$. crystal structure in $;(0\le \textrm x\le0.6)$ maintained space group Pnma with CaTiO_3 structure. The tiled and distorted $TiO_6$ was gradually released with the increase of x in $0\le \textrm x\le0.6$ .The structure was changed to a new space group of $Pmn2_1$ at the x value of 0.8. The relative dielectric constant $(\epsilon_r)$ of $(1-x)CaTiO_3-x(La_{1/3} Nd_{1/3})TiO_3$ ($(0\le \textrm x\le0.8)$) system was exponentially decreased by with the increased of x. The temperature coefficient of resonant frequency $(\tau_f)$ decreased with the increase of x in $0\le \textrm x\le0.6$ and then increased again at x=0.8 due to the change of crystal structure. The value of Q$\cdot f_o$ was 13800 (GHz) at x=0.2 and was very low under 2000 (GHz) in 0.4$\leq$x$\leq$0.8.

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Study on Burnability and Reactivity of High Al2O3 Content OPC Clinker for the Use of Industrial Waste (산업부산물 활용을 위한 고Al2O3 함량 OPC 클링커의 소성성 및 반응성에 관한 연구)

  • Kang, Bong-Hee;Choi, Jaewon;Ki, Tae-Kyoung;Kwon, Sang-Jin;Kim, Gyu-Yong
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.8 no.3
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    • pp.294-301
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    • 2020
  • This study evaluated the burnability and hydration reaction of clinker burned with high Al2O3 content OPC to apply large amounts of industrial by-products in the cement manufacturing process. Specifically, after preparing a clinker with a high C3A content by burning the OPC raw material with a high content of Al2O3 in a laboratory electric furnace, the burnability of the clinker was evaluated through XRD Rietveld analysis and polarization microscopy, and clinker hydration reactivity was reviewed through the Isothermal conduction calorimetry analysis and the cement compressive strength. As a result, the kiln burning temperature for the production of high Al2O3 content clinker lower, and the compressive strength was equal to or higher than OPC. Therefore it was confirmed the possibility to manufacturing energy-saving high Al2O3 content clinker using a large amount of industrial by-products.