• 한국광물학회지
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• 제14권2호
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• pp.128-136
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• 2001

흘란다이트 터널 구조내의 A자리 양이온인 $Ba^{2+}$ 이온을 $K^{+ }$ 이온이 치환하면서 결정의 구조에 어떠한 변화가 있는지 알아보기 위해 K-Ba 전구간 완전고용체로 치환된 7개의 합성 흘란다이트형 광물($K_{2x}$ $Ba_{1}$ -x/$Cr_2$$Ti_{6}$ $O_{16}$ , x=0, 0.1, 0.3, 0.5, 0.7, 0.9, 1.0)에 대하여 X선 회절분석과 리트벨트 구조분석법을 실시하였다. 리트벨트 계산 결과, 구조의 정밀도를 나타내는 R 지수값을 보면$ R_{exp}$에 대한 $R_{wp}$ 값($R_{wp}$ /$R_{exp}$ )은 15.77%/20.90%~14.74%/l9.37%의 범위를 보여주며, $R_{B}$ 값은 6.45~8.97%, S (GofF)값은 1.45~l.63으로 각각 계산되었다. 합성 홀란다이트는 K-Ba 전구간에서 Ba의 함량에 관계없이 모두 공간군 14/m을 가지며, 단위포의 크기는 a=10.1194(2) ~ 10.0599(2)$\AA$, c=2.9572(6)~2.9512(7)$\AA$, V=302.75~298.66$\AA^{3}$의 범위를 보여주며, K 함량이 50% 이상에서는 금홍석이 부산물로 합성되었다. 그 결과 A자리의 Ba와 K의 치환관계에서는 비록 단위포의 크기에 일정한 변화를 보여주었으나 구조적 변이에 영향을 주기에는 충분치 않은 것으로 밝혀졌다. 따라서 정방정계에서 대칭성이 낮은 단사정계로의 구조적 변이는 A자리에 대한 K-Ba 치환보다는 다른 양이온의 치환이나 B자리의 치환 등 다른 요인에 의할 것으로 생각된다.다.

• 한국결정학회지
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• 제9권1호
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• pp.48-52
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• 1998

Nd2O3, BaCo3, Co3O4를 출발물질로 하여 새로운 Nd3Ba5Co4O15상을 고상반응법에 의하여 합성하였다. 반응 온도는 1200℃ 로 하였고 열처리 중 반복적인 혼합을 실시하였다. Nd3Ba5Co4O15상의 결정구조는 분말 X-선회절법에 의한 데이터를 Rietveld법을 이용하여 정밀화하였다. 출발 모델은 Nd3.43Ba4.42Co2.23Al1.77O15의 결정구조를 따랐고 공간군 P63mc(186), 격자상수 a=11.636(5) Å, c=6.846(3) Å. 최종 신뢰도 R값은 Rwp=0.097, Rp=0.068로 나타났다. 이 상의 결정구조는 CoVICoIV3O15 클러스터로 구성되어 있고 이 클러스터는 CoVI 육면체가 3개의 CoIV 사면체와 corner sharing하는 형태를 보인다.

• Journal of Magnetics
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• 제14권2호
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• pp.86-89
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• 2009

Structural and magnetic properties of polycrystalline $CaFe_2O_4$ prepared by the solid state reaction method were studied using powder X-ray diffraction (XRD) and $M{\ddot{o}}ssbauer$ spectroscopy. The structure of $CaFe_2O_4$ belongs to an orthorhombic system (space group: Pnma) with the lattice parameters $a=9.2373\;{\AA}$, $b=3.0237\;{\AA}$, and $c=10.7124\;{\AA}$. Results of structural refinement indicate, however, that there are two slightly different iron sites in the sample. The $M{\ddot{o}}ssbauer$ spectrum at 4.2 K shows a hyperfine sextet with a hyperfine magnetic field and an isomer shift of 47.3 T and 0.36 mm/s, respectively. An examination of the spectrum revealed that the line widths of the spectral lines were not uniform. The degree of asymmetric line broadening decreases with increasing temperature, suggesting that the difference in the degree of crystalline distortions between two $FeO_6$ octahedra is eliminated as the temperature rises.

• 한국재료학회지
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• 제30권8호
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• pp.413-420
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• 2020

Lu₃Al_5-xGa_xO₁₂: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.

• 한국세라믹학회지
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• 제42권2호
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• pp.123-126
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• 2005

용매열법으로 출발물질의 농도를 변수로 차여 $BaTiO_3$ 분말을 합성하였다. 평균입자크기는 출발물질의 농도에 따라 비례하였는데 TiO_2를 기준으로 1/16M 농도에tj 59nm이었고 1/2M 농도에서는 89nm까지 증가하였다. 평균입자 크기가 89nm인 BT 분말에 대하여 리트벨트법에 의하여 분석한 결과 상분율은 정방정상 $75.5\%$이었고, 격자상수는 정방정상은 a=0.3999(nm), c=0.40319(nm)이고, 입방정상은 a=0.4015(nm)이었다. 이 분말을 $500^{\circ}C$ 1시간 열처리 후 TEM분석을 한 결과, 분말 내부에 수산 이온들이 거의 존재하지 않음을 확인하였다.

• 한국전기전자재료학회논문지
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• 제14권5호
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• pp.383-390
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• 2001

We have investigated the L $i_{1+x}$M $n_2$ $O_4$system as a cathode material for lithium rechargeable batteries. To improve the cycle performance of spinel LiM $n_2$ $O_4$ as the cathode of 4V class lithium secondary batteries, spinel phase L $i_{1+x}$M $n_2$ $O_4$(x=0, 0.025, 0.05, 0.075) was prepared at 75$0^{\circ}C$ for 48h. The preparation of L $i_{1+x}$M $n_2$ $O_4$ from L $i_2$ $O_3$ and Mn $O_2$ under air is studied. The compounds were synthesized by using solid-state reaction. Structural refinements were carried out with a Rietveld-refinement program. Electrochemical properties were examined using the Li/L $i_{1+x}$M $n_2$ $O_4$ cells. The capacity of L $i_{1+x}$M $n_2$ $O_4$ decreases with increases lithium content, while the cycle life improves. The initial discharge capacity are 118mAh/g and 116mAh/g for LiM $n_2$ $O_4$ decreases with increases lithium content, while the cycle life improves. The initial discharge capacity are 118mAh/g and 116mAh/g for LiM $n_2$ $O_4$ and L $i_{1.025}$M $n_2$ $O_4$, respectively.pectively.

• 대한금속재료학회지
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• 제48권3호
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• pp.262-267
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• 2010

$LiNi_{1-x}Mg_xO_2$(x=0, 0.025, 0.05, 0.075, 0.1) samples were synthesized by the solid-state reaction method. The crystal structure was analyzed by X-ray powder diffraction and Rietveld refinement. $LiNi_{1-x}Mg_xO_2$samples give single phases of hexagonal layered structures with a space group of R-3m. The calculated cation-anion distances and angles from the Rietveld refinement were changed with Mg contents in $LiNi_{1-x}Mg_xO_2$. The thicknesses of $NiO_2$ slabs were increased and the distances between the $NiO_2$ slabs were decreased with the increase in Mg contents in the samples. The electrical conductivities of sintered $LiNi_{1-x}Mg_xO_2$ samples were around $10^{-2}$ S/cm at room temperature. The electrochemical performances of $LiNi_{1-x}Mg_xO_2$were evaluated by coin cell test. Compared to $LiNiO_2$, $LiNi_{0.95}Mg_{0.05}O_2$ exhibited improved high-rate capability and cyclability due to the well-ordered layered structure by doping of Mg ion.

• The Journal of Advanced Prosthodontics
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• 제14권5호
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• pp.285-293
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• 2022

PURPOSE. This study evaluated the relationship among translucency, crystalline phase, grain size, and fracture toughness of zirconia. MATERIALS AND METHODS. Four commercial zirconia - Prettau^®Anterior^® (PA), Prettau^® (P), InCorisZI (ZI), and InCorisTZI (TZI)- were selected for this study. The bar specimens were prepared to determine fracture toughness by using chevron notched beam method with four-point bending test. The grain size was evaluated by a mean linear intercept method using a scanning electron microscope. X-ray diffraction and Rietveld refinement were performed to evaluate the amount of tetragonal and cubic phases of zirconia. Contrast ratio (CR) was measured to investigate the level of translucency. RESULTS. PA had the lowest fracture toughness among other groups (P < .05). In addition, the mean fracture toughness of P was significantly less than that of ZI, but there was no difference compared with TZI. Regarding grain size measurement, PA had the largest average grain size among the groups. P obtained larger grain size than ZI and TZI (P < .05). However, there was no significant difference between ZI and TZI. Moreover, PA had the lowest CR value compared with the other groups (P < .05). This means PA was the most translucent material in this study. Rietveld refinement found that PA presented the greatest percentage of cubic phase, followed by TZI, ZI, and P, respectively. CONCLUSION. The different approaches are used by manufacturers to fabricate various types of translucent zirconia with different levels of translucency and mechanical properties, which should be concerned for material selection for successful clinical outcome.

• Bulletin of the Korean Chemical Society
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• 제34권6호
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• pp.1679-1683
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• 2013

Intergrowth perovskite type complex oxides $La_{0.8}Ln_{0.2}Sr_2MnCrO_{7-{\delta}}$ (Ln=La, Nd, Gd, and Dy) have been synthesized by sol-gel method. Rietveld profile analysis shows that the phases crystallize with tetragonal unit cell in the space group I4/mmm. The unit cell parameters a and c decrease with decreasing effective ionic radius of the lanthanide ion. The magnetic studies suggest that the ferromagnetic interactions are dominant due to $Mn^{3+}$-O-$Mn^{4+}$ and $Mn^{3+}$-O-$Cr^{3+}$ double exchange interactions. Both Weiss constant (${\theta}$) and Curie temperature ($T_C$) increase with decreasing ionic radius of lanthanide ion. It was found that the transport mechanism is dominated by Mott's variable range hopping (VRH) model with an increase of Mott localization energy.

• 한국세라믹학회지
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• 제42권5호
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• pp.299-303
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• 2005

The crystal structure and ferroelectricity of the $(1-x)BiFeO_3\;(BF)-xPbTiO_3$ (PT) ceramic system with the addition of $DyFeO_3$ (DF) have been investigated for attaining a high temperature piezoelectric material. This study is focused on the relation between crystal structure and ferroelectric property with the addition of DF over the phase boundary in the (1-x)BF-xPT system. Hysteresis curves of polarization-electric field at room temperature have been measured. The X-ray and neutron diffraction data were analyzed by the rietveld refinement method. The addition of 0.1 mole DF into BF-PT system greatly increases the ferroelectric remanant polarization Pr values, e.g. 17 ${\mu}C/cm^2$ in 0.6BF-yDF-(0.4-y)PT and 31${\mu}C/cm^2$ in 0.5BF-yDF-(0.5.y)PT, respectively. The improved Pr value has been discussed in relation with crystal structure and electrical property.