• Nuclear Engineering and Technology
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• v.54 no.5
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• pp.1560-1569
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• 2022

Liquid fueled molten salt reactors (MSRs) have seen renewed interest because of their inherent safety features, higher thermal efficiency and potential for efficient thorium utilisation for power generation. Thorium fluoride is one of the salts used in liquid fueled MSRs employing Th-U cycle. In the present study, ThF₄ was prepared by hydro-fluorination of ThO₂ using anhydrous HF gas. Process parameters viz. bed depth, hydrofluorination time and hydrofluorination temperature, were optimized for the preparation of ThF₄ in a static bed reactor setup. The products were characterized with X-Ray diffraction and experimental conditions for complete conversion to ThF₄ were established which also corroborated with the yield values. Hydrofluorination of ThO₂ at 450 ℃ for half an hour at a bed depth of 6 mm gave the best result, with a yield of about 99.36% ThF₄. No unconverted oxide or any other impurity was observed. Rietveld refinement was performed on the XRD data of this ThF₄, and Chi2 value of 3.54 indicated good agreement between observed and calculated profiles.

• 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 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.26 no.1
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• pp.27-34
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• 2013

X-ray powder diffraction is one of the most powerful techniques for qualitative and quantitative analysis of crystalline compounds. Thus, there exist a number of different methods for quantifying mineral mixtures using X-ray diffraction pattern. We present here the use of Rietveld and PONKCS (partial or no known crystal structure) methods for quantification of amorphous and crystallized mineral phases in synthetic mixtures of standard minerals (amorphous silica, quartz, mullite and corundum). Pawley phase model of amorphous silica was successfully built from the pattern of 100 wt% amorphous silica and internal standard-spiked samples by PONKCS approach. The average of absolute bias for quantities of amorphous silica was 1.85 wt%. The larger bias observed for lower quantities of amorphous silica is probably explained by low intensities of diffraction pattern. Averages of absolute bias for minerals were 0.53 wt% for quartz, 0.87 wt% for mullite and 0.57 wt% for corundum, respectively. The PONKCS approach achieved improved quantitative results compared with classical Rietveld method by using an internal standard.

• Journal of the Mineralogical Society of Korea
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• v.13 no.3
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• pp.164-170
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• 2000

Neutron single crystal and powder diffraction techniques have been applied to the structure analysis of yttria-stabilized zirconium, Z $r_{0.73}$ $Y_{0.27}$ $O_{1.87}$., prepared by the skull-melting method. The crystal structure has been determined to be cubic symmetry, space group Fm/equation omitted/ with a=5.155(2)$\AA$, V=136.99(5)$\AA$, Z=4, and R(F)=5.65%, $\omega$R(I)=10.57% for 70 integrated intensities of Bragg Peaks observed from single crystal of Z $r_{0.73}$ $Y_{0.27}$ $O_{1.87}$. The stabilizer atoms randomly occupy the zirconium sites and there are displacements of oxygen atoms with amplitudes of $\Delta$/a~0.033 and 0.11 along <110> and <100> directions from the ideal positions of the fluorite structure, respectively. There are no significant differences in crystallographic data between the single crystal and powder studies. Diffraction pattern after Rietveld refinement, using neutron powder data, has shown the evidence of a tetragonal impurity phase, or a slight tetragonal distortion.

• Journal of the Mineralogical Society of Korea
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• v.19 no.4 s.50
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• pp.363-381
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• 2006

Mineral compositions of granitic rocks from Geochang, Pocheon, Iksan, and China were obtained by the modal analysis, CIPW norm calculations, and Rietveld quantitative analysis for stone specification of the Geochang granitic rocks. The Geochang granitic rocks show grey to dark in color and medium grained porphyritic texture. They mainly consist of quartz, plagioclase, alkali feldspar, and biotite. Among three different method for determining the mineral compositions of granitic rocks, normative compositions using X-ray fluorescence data are not appropriate for representing real mineral composition. Rietveld quantitative analysis using X-ray powder diffraction data is proved better method to determine exact mineral compositions than modal analysis using microscopic observation. Q-A-P diagram shows that the Geochang granitic rocks are typical granodiorite, whereas the granitic rocks of Pocheon, Iksan, and China are monzogranite, monzogranite to granodiorite, and granodiorite, respectively. Compared to China ones, the Geochang granitic rocks are nearly close to each other in mineral composition.

• Journal of the Korean Electrochemical Society
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• v.6 no.1
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• pp.1-5
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• 2003

[ $LiNi_{1-x}Co_xO_2\;(x=0.0\~1.0)$ ] powders were synthesized by citrate method, and their crystal structures and electrochemical performance as the cathode material in Li secondary batteries were analyzed. X-ray diffraction analysis revealed that all the samples carry a single phase regardless of the Co substitution. The results of Rietveld refinement suggested that the crystal structure of solid solutions varies according to the Co substitution. When the Co substitution is low $(x=0.3\~0.5)$, the solid solutions carry a cubic-like structure with a relatively small value in the ratio of lattice parameters (c/a). The solid solutions made with a higher Co substitution (x=0.7), however, exhibit a layered structure with a higher c/a ratio. This difference was also observed in the electrochemical voltage spectroscopy (EVS) profiles, whereby the Co component in scarcely substituted materials shows a charging reaction at $3.7V\;(vs.\;Li/Li^+)$, but in the heavily substituted ones at 3.92V.

• Korean Journal of Materials Research
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• v.5 no.6
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• pp.748-753
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• 1995

Solid solution of NaNb $O_3$70 mol% and SrTi $O_3$30 mol% was single phase. A broad dielectric peak was found at about l00K. Crystal structure was analysed at room temperature and 12K using Rietveld analysis. The unit cell was assigned to have a a doubled lattice parameter of simple perovskite sturcture at room temperatue, the structure was orthorombic with space group Pmmn. At 12K, the structure was also orthorombic with space group Pnma. This structure change with temperature was due to the distortion of oxygen octahedron. This distortion of oxygen octahedron was made by the decrease of (Ti, Nb)-O bounds length with no variation of (Ti, Nb)-O-(Ti, Nb) bound angle. Therefore the broad dielectirc peak about l00K was attributed to the structural change casued by oxygen octahedron distortion.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.30 no.6
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• pp.244-250
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• 2020

β-Tricalcium phosphate (β-TCP, Ca3(PO4)2) is a kind of biodegradable calcium phosphate ceramics with chemical and mineral compositions similar to those of bone. It is a potential candidate for bone repair surgery. To improve the bioactivity and osteoinductivity of β-TCP, various ions doped calcium phosphate have been studied. Among them, Iron is a trace element and its deficiency in the human body causes various problems. In this study, we investigated the effect of Fe ions on the structural variation, degradation behavior of β-TCP. Fe-doped β-TCP powders were synthesized by the coprecipitation method, and the heat treatment temperature was set at 925 and 1100℃. The structural analysis was carried out by Rietveld refinement using the X-ray diffraction results. Fe ions existed in a different state (Fe2+ or Fe3+) with different heat treatment temperatures, and the substitution sites (Ca-(4) and Ca-(5)) also changed with temperature. The degradation rate was fastest at Fe-doped β-TCP with heated at 1100℃. The cell viability behavior was also enhanced with the substitution of Fe ions. Therefore, the substitution of Fe ion has accelerated the degradation of β-TCP and improved the biocompatibility. It could be more utilized in biomedical devices.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.33 no.5
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• pp.174-180
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• 2023

Porcelain (white ware, celadon ware) coated with a ferrous sulfate and ferrous/cobalt sulfate was sintered at 1250℃. The specimens were investigated by HR-XRD, FE-SEM, HR-EDS, and UV-vis spectrophotometer. Through X-ray rietveld quantitative analysis, quartz and mullite were found to be the main phases for white ware, and mullite and plagioclase were found to be the main phases for celadon ware. When the pigment of ferrous/cobalt sulfate was applied, were identified as an andradite phase for celadon ware and a spinel phase for the white ware, and the amorphous phase, respectively. The L^* value, which was the brightness of the specimen, was 72.01, 60.92 for white ware and celadon ware, respectively. The ferrous and ferrous/cobalt pigment coated porcelain had L^* values of 44.89, 52.27 for white ware and celadon ware, respectively; with a^* values of 2.12, 1.40, an d at b^* values of 1.45 and 13.79. As for the color of the specimens, it was found that the L^* value was greatly affected by the white ware, and the b^* value differed greatly depending on the clay. It was thought to be closely related to the production of the secondary phase such as Fe₂O₃ and andradite phase produced in the surface layer.