• Journal of the Korean Chemical Society
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• v.58 no.2
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• pp.239-241
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• 2014

• Bulletin of the Korean Chemical Society
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• v.30 no.1
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• pp.183-187
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• 2009

The structure of nano-crystalline $MnFe_2O_4$ was determined and refined with electron powder diffraction data employing the Rietveld refinement technique. A nano-crystalline sample (with average crystal size of about 10.9 nm) was characterized by selected area electron diffraction in an energy-filtering transmission electron microscope operated at 120 kV. All reflection intensities were extracted from a digitized image plate using the program ELD and then used in the course of structure refinements employing the program FULLPROF for the Rietveld analysis. The final structure was refined in space group Fd-3m (# 227) with lattice parameters a=8.3413(7) $\AA$. The reliability factors of the refinement are $R_F$=7.98% and $R_B$=3.55%. Comparison of crystallographic data between electron powder diffraction data and reference data resulted in better agreement with ICSD-56121 rather than with ICSD-28517 which assumes an initial structure model.

• Bulletin of the Korean Chemical Society
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• v.16 no.2
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• pp.120-125
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• 1995

Solid solutions of Pr2-xBaxNiO4±δ with K2NiF4-type structure were prepared in air and characterized by powder X-ray diffraction, Rietveld refinements, iodometry titrations, and conductivity measurements. The range of the solid solution was 0 ≤ x < 0.5. The crystal structure changes from orthorhombic (Fmmm) for x ≤ 0.1 to pseudo-tetragonal (I4/mmm) for x ≥ 0.2. The orthorhombic structure of x=0.1 transforms to tetragonal at low temperature. The bond distances obtained from the Rietvel analyses did not vary significantly with the Ba content except that of Ni-O (parallel to the c-axis) which showed an abrupt increase from x=0.1 to 0.2. The excess oxygen content (δ) decreases from 0.241 to 0.03 with increasing substituted Ba contents within the solution range. The samples are all semiconductors at the temperature range 4 < T < 300 K.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.14 no.5
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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.

• Journal of the Mineralogical Society of Korea
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• v.16 no.3
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• pp.215-222
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• 2003

The Rietveld structure refinement for the natural trioctahedral mica, phlogopite-1M (Parker Mine, Quebec, Canada) has been done by high resolution neutron powder diffraction at $25^{\circ}C$ and -263$^{\circ}C$. The structural formula of phlogopite determined by electron probe microanalysis is $K_2$(M $g_{4.46}$F $e_{0.83}$A $l_{0.34}$ $Ti_{0.22}$)(S $i_{5.51}$A $l_{2.49}$) $O_{20}$(O $H_{3.59}$ $F_{0.41}$). Cell parameters are a=5.30∼5.31 $\AA$, b=9.18∼9.20 $\AA$, c=10.18∼10.21 $\AA$, $\beta$=100.06∼100.08$^{\circ}$. Refinements converged to R values in the range of $R_{p}$=2.35%, $R_{wp}$=3.01%, respectively. In this study, the OH bond length is calculated to 0.93 $\AA$ at room temperature and 1.03 $\AA$ at -263$^{\circ}C$, and the angles between OH vector and (001) plane are obtained 93.4$^{\circ}$∼93.6$^{\circ}$. The decrease in the length of OH with the increase in temperature should be due to the hydrogen bonding in the structure of phogopite.e.e.f phogopite.e.e.

• Journal of the Mineralogical Society of Korea
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• v.19 no.1 s.47
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• pp.15-29
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• 2006

Synthetic Mn-tourmalines (tsilaisite) were obtained by hydrothermal synthesis under the condition of 2 Kbar, $375{\sim}700^{\circ}C$, and 50 day-run-time with complete substitution of Mg in dravite by Mn (Mn%=0, 25, 50, 75, and 100%). They are all 6 samples containing Mn-tourmaline with some amounts of albite, spessartine, rhodocrosite, phlogopite etc, showing different synthetic condition of temperature and Mn composition. Synthetic Mn-tourmalines are of site deficiency in X-site ($0.53{\sim}0.68$) more than that of natural ones (approx. $0.2{\sim}0.3$) and show Mn cations occupying Y-site less than expected with initial experiments, leading to failure in synthesis of end-member tsilaisite. Rietveld structural refinements reveal that $R_{wp}$ ($R_{p}/R_{exp}$) is in the range of 13.35 and 18.62%, $R_{B}$ and S (CofF) are $4.85{\sim}6.25%$ (S-18: 8.57%), $1.31{\sim}1.59$ (S-18: 1.81), respectively. Unit cell parameters (space group R3m, z=3) are ${\alpha}=15.8994\;{\AA}$ and $c=7.1846\;{\AA}$ in average (S-18: ${\alpha}=15.9491\;{\AA},\;c=7.1773\;{\AA}$). Average bond lengths of and are $2.67{\sim}2.69\;{\AA}$ (S-18: $2.65\;{\AA}$) and $2.00{\sim}2.02\;{\AA}$ (S-18: $1.96\;{\AA}$), respectively. Ditrigonality (${\delta}$) are in the range of 0.022 and 0.031 (S-18: 0.061), indicating degrading symmetry with increase of Mn content.

• Journal of the Korean Chemical Society
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• v.47 no.6
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• pp.614-618
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• 2003

$Sr_2Ru_{1-x}Cu_xO_{4-y}(0.0{\le}x{\le}0.5)$ compounds were prepared using a conventional solid state reaction. Based on the Rietveld refinements of X-ray diffraction results, it is revealed that $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds are the single phases with K2NiF4 type tetragonal system in the range of 0=x=0.3, while the mixed phases of$Sr_2RuO_4$ and $Sr_2CuO_3$ in the range of $0.4{\le}x{\le}0.5$. By means of X-ray photoelectron spectroscopy, the valence states of Ru and Cu in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, have been confirmed to 4+ and 2+, respectively. The bond length difference between $Ru-O_1 ({\times}4)\;and\;Ru-O_2 ({\times}2)\;in\;RuO_6$ octahedron is gradually decreased with increasing Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, which results in the lower c/a ratio. So, it might be assured that the variation of local symmetry of $RuO_6$ octahedron is very closely related to the transporting property of $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds. The behavior of resistivity discloses that the metallic property in $Sr_2RuO_4$ changes into the semiconducting one in proportion to the Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$.