• Journal of the Mineralogical Society of Korea
• /
• v.14 no.2
• /
• pp.128-136
• /
• 2001

The K-Ba complete solid solution of 7 synthetic hollandite-type minerals ($K_{2x}$ $Ba_{1-x}$ $Cr_2$/$Ti_{6}$ $O_{16}$ , x=0, 0.1, 0.3, 0.5, 0.7, 0.9, 1.0, respectively) are studied by the X-ray powder diffraction and Rietveld refinement to find structural transformation during substitution of $Ba^{2+}$ by $K^{+}$ in A site of the tunnel structure of hollandite. Rietveld indices indicate that $R_{wp}$ with respect to $R^{exp}$ ($R_{wp}$ $R_{exp}$ ) are in the range of 15.66%/20.90% and 14.74%/l9.37%, $R_{B}$ and S(Goodness of Fitness) are 6.45~8.97%, 1.45~1.63, respectively. Unit cell parameters of synthetic hollandites, space group 14/m, are a=10.1194(2)~10.0599(2)$\AA$, c=2.9572(6)~2.9512(7)$\AA$, and V=302.75~298.66$\AA^{3}$. Rutile formed as an impurity in those with more than 50% K contents in hollandite series. Substitution of Ba by K ion in a tunnel structure results in constant decrease of cell parameters, but is not sufficient enough to change the hollandite structure. Our data indicate that transformation of tetragonal 14/m to lower symmetry of monoclinic 12/m in hollandite structure may at least be affected by other cation substitution in same A site and/or by cation substitution in B site.

• Korean Journal of Crystallography
• /
• v.9 no.1
• /
• pp.48-52
• /
• 1998

The new Nd3Ba5Co4O15 phase was synthesized with Nd2O3, BaCO3, and Co3O4 by solid state reaction at 1200℃ with intermittent grinding. The crystal structure of Nd3Ba5Co4O15 has been refined on X-ray diffraction powder data by means of Rietveld method. The starting model was based on the Nd3.43Ba4.42Co2.23Al1.77O15 structure. The crystal system was hexagonal, space group P63mc(186), a=11.629(3) Å, c=6.842(2) Å. Final R values were Rwp=0.097 and Rp=0.068. The structure consists of clusters of CoVICoIV3O15 in which a CoVI octahedron shares corners with 3CoIV tetrahedra.

• Journal of Magnetics
• /
• v.14 no.2
• /
• pp.86-89
• /
• 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.

• Korean Journal of Materials Research
• /
• v.30 no.8
• /
• pp.413-420
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.42 no.2 s.273
• /
• pp.123-126
• /
• 2005

Barium Titanate (BT) powders were synthesized by solvothermal method with an ethanol as a solvent. The average particle size was increased with the feedstock concentration: the size was 59 nm at $6.25{\times}10^{-2}$ M and 89 nm at 0.5 M. The sample obtained at 0.5 M concentration was analysed by Rietveld refinement and the mole fraction of tetragonal phase was $75.5\%$ and lattice parameter of tetragonal phase was a=0.3999 (nm), c=0.4032 (nm), and cubic phase was a=0.4015 (nm). TEM analysis for the samples with condition of annealing at $500^{\circ}C$ for I h showed that hydroxyl ions on oxygen sites were not found for these experimental conditions.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.14 no.5
• /
• pp.383-390
• /
• 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.

• Korean Journal of Metals and Materials
• /
• v.48 no.3
• /
• pp.262-267
• /
• 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
• /
• v.14 no.5
• /
• pp.285-293
• /
• 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
• /
• v.34 no.6
• /
• pp.1679-1683
• /
• 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.

• Journal of the Korean Ceramic Society
• /
• v.42 no.5 s.276
• /
• pp.299-303
• /
• 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.