• Journal of Magnetics
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• v.14 no.2
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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.

• Journal of Powder Materials
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• v.11 no.3
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• pp.233-241
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• 2004

In this study, bottom-up type powder processing and top-down type SPD (severe plastic deformation) approaches were combined in order to achieve both full density and grain refinement of Al-20 wt% Si powders without grain growth, which was considered as a bottle neck of the bottom-up method using the conventional powder metallurgy of compaction and sintering. ECAP (Equal channel angular pressing), one of the most promising method in SPD, was used for the powder consolidation. The powder ECAP processing with 1, 2, 4 and 8 passes was conducted for 10$0^{\circ}C$ and 20$0^{\circ}C$ It was found by microhardness, compression tests and micro-structure characterization that high mechanical strength could be achieved effectively as a result of the well bonded powder contact surface during ECAP process. The SPD processing of powders is a viable method to achieve both fully density and nanostructured materials.

• International Journal of Korean Welding Society
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• v.3 no.2
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• pp.46-52
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• 2003

The refinement of microstructure and phase transformation near the interface of pure copper/carbon steel dissimilar metals joints with various friction welding parameters have been studied in this paper. The microstructure of copper and carbon steel joints were changed to be a finer grain compared to those of the base metals due to the frictional heat and plastic deformation. The microstructure of copper side experienced wide range of deformed region from the weld interface and divided into very fine equaxied grains and elongated grains. Especially, the microstructures near the interface on carbon steel were transformed from ferrite and pearlite dual structure to fine ferrite, grain boundary pearlite and martensite due to the welding thermal cycle and rapid cooling rate after welding. These microstructures were varied with each friction welding parameters. The recrystallization on copper side is reason for softening in copper side and martensite transformation could explain the remarkable hardening region in carbon steel side.

• Economic and Environmental Geology
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• v.34 no.1
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• pp.1-12
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• 2001

The crystal structure of biotite-1M from Bancroft, Ontario, was determined by Rietveld refinement method using high-resolution neutron powder diffraction data at -26.3$^{\circ}C$, 2$0^{\circ}C$, 30$0^{\circ}C$, $600^{\circ}C$, 90$0^{\circ}C$. The crystal structure has been refined to a R sub(B) of 5.06%-11.9% and S (Goodness of fitness) of 2.97-3.94. The expansion rate of a, b, c unit cell dimensions with elevated temperature linearly increase to $600^{\circ}C$. The expansivity of the c dimension is $1.61{\times}10^{40}C^{-1}$, while $2.73{\times}10^{50}C^{-1}$ and $5.71{\times}10^{-50}C^{-1}$ for the a and b dimensions, respectively. Thus, the volume increase of the unit cell is dominated by expansion of the c axis as increasing temperature. In contrast to the trend, the expansivity of the dimensions is decreased at 90$0^{\circ}C$. It may be attributed to a change in cation size caused by dehydroxylation-oxidation of $Fe^{2+}$ to $Fe^{3+}$ in vacuum condition at such high temperature. The position of H-proton was determined by the refinement of diffraction pattern at low temperature (-2.63$^{\circ}C$). The position is 0.9103${\AA}$ from the O sub(4) location and located at atomic coordinates (x/a=0.138, y/b=0.5, z/c=0.305) with the OH vector almost normal to plane (001). According to the increase of the temperature, $\alpha$* (tetrahedral rotation angle), $t_{oct}$ (octahedral sheet thickness), mean distance increase except 90$0^{\circ}C$ data. But the trend is less clearly relative to unit cell dimension expansion because the expansion is dominant to the interlayer. Also, ${\Psi}$ (octahedral flattening angle) shows no trends as increasing temperature and it may be because the octahedron (M1, M2) is substituted by Mg and Fe.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.28 no.4
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• pp.152-158
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• 2018

PVT (Physical Vapor Transport) method has advantages in producing high quality, large scale wafers where many researches are being carried out to commercialize nitride semiconductors. However, complex process variables cause various defects when it had non-equilibrium growth conditions. Annealing process after crystal growth has been widely used to enhance the crystallinity. It is important to set appropriate temperature, pressure, and annealing time to improve crystallinity effectively. In this study, the effect of the annealing conditions on the crystalline structure variation of the AlN single crystal grown by PVT method was investigated with synchrotron whitebeam X-ray topography, electron backscattered diffraction (EBSD), and Rietveld refinement. X-ray topography analysis showed secondary phases, sub-grains, impurities including carbon inclusion in the single crystal before annealing. EBSD analyses identified that sub-grains with slightly tilted basal plane appeared and the overall number of grains increased after the annealing process. Rietveld refinement showed that the stress caused by the temperature gradient during the annealing process between top and bottom in the hot zone not only causes distortion of grains but also changes the lattice constant.

• 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.

• Journal of the Korean Chemical Society
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• v.34 no.1
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• pp.1-9
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• 1990

Cholesteryl pentanoate $(C_{32}O_2H_{54})$ is orthorhombic, space group $P2_12_12_1$, with a = 21.930(3), b = 21.404(3), c = 6.419(5) $\AA$, Z = 4, V = 3012.8(5)$\AA$$^3$, $D_c$ = 1.04 g$cm^{-3}$, ${\lambda}(Mo\; K{\alpha}$ = 0.71069 $\AA$, $\mu$ = 0.58 $cm^{-1}$, F(000) = 1048, T = 298, R = 0.086 for 1502 unique observed reflections with I > 1.0 $\sigma$ (I). The structure was solved by direct methods and refined by cascade diagonal least-squares refinement. The C-H bond lengths and the methyl groups are fixed and refined as their ideal geometry. A comparison with other cholesteryl esters gives normal structure for the tetracyclic ring, while the tail regions of the side chain and the ester group which stands on end, show a variation from their normal values, presumably due to thermal effects. The molecules are stacked together by non-bonded van der Waals forces with the shortest intermolecular distance of 3.529 $\AA$.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.15 no.1
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• pp.67-74
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• 2002

A phosphor for Plasma Display Panel, BaMgAl$_{10}$ O$_{17}$ :Eu$^{2+}$, showing a blue emission band at about 450nm was prepared by a solid-state reaction using BaCO$_3$, $Al_2$O$_3$, MgO, Eu$_2$O$_3$ as starting materials wish flux AlF$_3$. The study of the behaviour of Eu in BAM phosphor was carried out by the photoluminescence spectra and the Rietveld method with X-ray and neutron powder diffraction data to refine the structural parameters such as lattice constants, the valence state of Eu, the preferential site of Mg atom and the site fraction of each atom. The phenomenon of the concentration quenching was abound 2.25~2.3wt% of Eu due to a decrease in the critical distance for energy transfer of inter-atomic Eu. Through the combined Rietveld refinement, R-factor, R$_{wp}$, was 8.11%, and the occupancy of Eu and Mg was 0.0882 and 0.526 at critical concentration. The critical distance of Eu$^{2+}$ in BAM was 18.8$\AA$ at 2.25% Eu of the concentration quenching. Furthermore, c/a ratio was decreased to 3.0wt% and no more change was observed over that concentration. The maximum entropy electron density was found that the modeling of $\beta$-alumina structure in BaMgAl$_{10}$ O$_{17}$ :Eu$^{2+}$correct coincided showing Ba, Eu, O atoms of z= 1/4 mirror plane.e.ane.e.

• Bulletin of the Korean Chemical Society
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• v.15 no.10
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• pp.891-896
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• 1994

Reactions of mer, trans-$Re({\equiv}NC_6H_5)(PPh_3)_2Cl_3$, I, with $PMe_3$ and $P(OMe)_34 at room temperature, led to mer, trans-$Re({\equiv}NC_6H_5)(PPh_3)(PMe_3)Cl_3$, II, and fac-$Re({\equiv}NC_6H_5)(PPh_3)(P(OMe)_3)Cl_34, III, respectively. The crystal structures of II and III were determined through X-ray diffraction. Ⅱ crystallizes in the orthorhombic system, space group $Pna2_1$ with cell parameters a=19.379(4) ${\AA}$, b=11.867(2) ${\AA}$, c = 12.676(3) ${\AA}$, and Z = 4. Least-squares refinement of the structure led to a $R(wR_2)$ factor of 0.0251 (0.0621) for 2203 unique reflections of $I>2{\sigma}(I)$ and for 306 variables. III crystallizes in the monoclinic system, space group $P2_1/n$ with cell parameters a=11.399(3) ${\AA}$, b=14.718(4) ${\AA}$, c=17.558(5) ${\AA}$, ${\beta}=97.79(2){\circ}$, and Z=4. Least-squares refinement of the structure led to a $R(wR_2)$ factor of 0.0571 (0.1384) for 3739 unique reflections of $I>2{\sigma}(I)$ and for 344 variables. Structural studies showed that the relative orientations of the two phosphines in both complexes are different, probably due to the differences in the coordinating abilities between $PMe_3$ and $P(OMe)_3$ to the 5-coordinate fluxional intermediate.

• 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.