• 제목/요약/키워드: rietveld analysis

검색결과 84건 처리시간 0.024초

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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    • 제33권6호
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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.

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

  • 최상준;권순주
    • 한국자기학회지
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    • 제6권2호
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    • pp.73-79
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    • 1996
  • Y형 육방정 산화철$(Ba_{2}Me_{2}Fe_{12}O_{22}:Me=천이금속)$은 천이 금속으로 Co와 Zn가 포함된 경우 양호한 고주파 특성을 보이는 것으로 알려져 있다. 따라서, 결정 구조 내에 이들의 분포 상태를 파악하는 것이 중요하다. 본 논문에서는 엄밀한 성분 분석, X-선 회절 분석, 자기 특성 분석을 통하여 확인된 $Co_{2}Y$$Co_{1.6}Zn_{0.4}Y$시료에 대한 $M\"{o}ssbauer$ 분광 분석 결과로부터 다음과 같은 결론을 제시하였다. (1) Co는 주로 육방정 산화철의 S-block에 위치한 4배위 자리 $(6c_{IV})$와 S-, T-block 경계의 6배위자리(18h VI)에 들어간다. (2) Co의 일부를 Zn으로 치환하여도, Fe의 분포에는 큰 영향을 미치지 않는다.

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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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    • 제73권10호
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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
    • 한국결정성장학회:학술대회논문집
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    • 한국결정성장학회 1997년도 Proceedings of the 12th KACG Technical Meeting and the 4th Korea-Japan EMGS (Electronic Materials Growth Symposium)
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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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리튬 2차 전지용 LiCo1-XMgxO2(x=0.03)의 결정구조, 전기전도도 및 전기화학적 특성 (Crystal Structures, Electrical Conductivities and Electrochemical Properties of LiCo1-XMgxO2(x=0.03) for Secondary Lithium Ion Batteries)

  • 김호진;정우창;정연욱;이준형;김정주
    • 한국세라믹학회지
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    • 제42권9호
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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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    • 제30권11호
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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.

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

  • 조경호;고영호;서창의;김광주
    • 한국세라믹학회지
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    • 제48권5호
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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
    • 한국세라믹학회지
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    • 제53권2호
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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.

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

  • 조남웅;성경필;문종하;최주현
    • 한국결정성장학회지
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    • 제8권3호
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    • pp.478-486
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    • 1998
  • $CaCO_3,\;LaO_3,\;Nd_2O_3\;TiO_2의 혼합물을 1673K에서 소결하여 마이크로파 유전체 세라믹스재료로 응용이 가능한 (1-x)$CaTiO_3-x(La_{1/3}Nd_{1/3}TiO_3\;(0\letextrm x\le0.8)$계를 합성하였다. (1-x))$CaTiO_3-x(La_{1/3}Nd_{1/3}TiO_3\;(0\lex\le0.8)$계의 격자 정수는 x가 증가함에 따라 증가하였다. XRD의 Rietveld profile-analysis를 통하여 (1-x))$CaTiO_3-x(La_{1/3}Nd_{1/3}TiO_3\;(0\le \textrm {x} \le0.8)$계의 결정구조를 해석하였다. $0\le \textrm {x}\le0.8$의 모든 영역에서 양이온 $La^{3+},Nd^{3+}$$Ca^{2+}$ 자리에 점유하였다. x=0.6까지는 $CaTiO_3$와 같은 공간군 Pnma를 그대로 유지하였으며, x가 증가함에 $TiO_6$의 비틀림과 변형은 점차 감소하였다. x=0.8에서는 새로운 공간군 $Pmn2_1$으로 결정구조의 변화를 보였다. (1-x)$CaTiO_3-x(La_{1/3}Nd_{1/3}TiO_3\;(0\le \textrm {x}\le0.8)$계의 비유전율($\epsilon$r)은 x가 증가함에 따라 지수 함수적으로 감소하였다. 공진 주파수의 온도계수($\tau_f$)는 x=0.6까지 증가함에 따라 감소하였으나 x=0.8에서는 결정구조의 변화와 더불어 다시 증가하였다. Q.$\tau_f$값은 x=0.2에서는 13800(GHz)을 나타낸 후 0$0.4\le \textrm {x}\le0.8$ 영역에서는 2000 (GHz)의 매우 낮은 값을 나타내었다.

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

  • 강봉희;최재원;기태경;권상진;김규용
    • 한국건설순환자원학회논문집
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    • 제8권3호
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    • pp.294-301
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    • 2020
  • 본 연구에서는 클링커의 고Al2O3화를 통한 에너지 절감형 시멘트 제조 가능성을 확인하기 위해, Al2O3 함량이 높은 OPC 조합원료를 실험실 전기로에서 소성하여 C3A 함량이 높은 클링커를 제조한 후 XRD 리트벨트 분석 및 광학 현미경을 통해 클링커의 소성성을 평가하고, 제조된 클링커에 혼합재를 첨가하여 얻어진 시멘트의 미소수화열 및 압축강도 측정을 통해 시멘트 반응성을 평가하고자 하였다. 그 결과 Al2O3 함량을 일반 OPC보다 증가시켜 제조한 시멘트는 OPC에 비해 소성성이 뛰어나 시멘트 제조 에너지 절감에 기여할 수 있으며, OPC에 비해 C3A(alite) 광물의 함량이 감소하였음에도 불구하고 압축강도가 오히려 향상되는 등 긍정적으로 작용할 수 있다. 유동성 저하, 수화열 증가와 같은 문제에 대해서도 석고 첨가량 및 분말도 조정, 혼합재 첨가와 같은 방법으로 제어할 수 있을 것으로 기대되어 적극적인 연구가 필요하다.