• 한국재료학회지
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• 제6권5호
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• pp.504-514
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• 1996

고상반응법과 sol-gel법으로 제조된 NASICON의 상온과 25$0^{\circ}C$에서의 X선 회절 데이터를 리트벨트 분석을 행하였다. monoclinic에서 rhombohedral로 상전이가 일어나도 원자들의 변위는 매우 작았다. 이들 상간의 ZrO6 팔면체와 Si(P)O4 사면체고 구성된 골격은 다소 다르게 나타남으로 인하여 Na 이온의 자리도 변하였다. 이들 방법으로 제조된 NASICON은 Zr이 부족한 비화학양론 화학식, Na 1+x+4yZr2-xSixP3-xO12으로 표현될 수 있었다. 제조법에 따라 Na 이온들의 자리 점유율이 변화하였다. 상온에서는 Na(1)과 Na(3)자리의 자리 점유율의 합이 거의 1에 가까웠으나, 25$0^{\circ}C$에서는 Na(1)과 mid Na 자리를 단위 화학식 당 한 개를 약간 상회하는 Na 이온이 점유하였다. 상온과 25$0^{\circ}C$에서의 Na 이온의 이동 경로가 다름을 알 수 있었다. 또한 25$0^{\circ}C$에서는 Na(1)자리와 Na(2)자리 사이에 mid Na가 존재하며, 이 자리가 Na 이온의 이동에 중요한 역할을 함을 알 수 있었다.

• Computers and Concrete
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• 제19권1호
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• pp.19-31
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• 2017

This paper uses modelling and experiment to perform a quantitative analysis for the gypsum and ettringite formations in cement pastes subjected to sulfate attack. Firstly, based on Fick's law and chemical reaction kinetics, a diffusion model of sulfate ions in cement pastes is proposed, and then the model of the gypsum and ettringite formations is established to analyze its contents in cement pastes with corrosion time. Secondly, the corrosion experiment of the specimens with cement pastes immersed into 2.5%, 5.0% and 10.0% $Na_2SO_4$ solutions are carried out, and by using XRD-Rietveld method, the phases of powder samples from the specimens are quantitatively analyzed to obtain the contents of gypsum and ettringite in different surface depth, solution concentration and corrosion time. Finally, the contents of gypsum and ettringite calculated by the models are compared with the results from the XRD experiments, and then the effects of surface depth, corrosion time and solution concentration on the gypsum and ettringite formations in cement pastes are discussed.

• 한국광물학회지
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• 제9권1호
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• pp.43-53
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• 1996

The detailed crystal chemistry of ilmenite from the Hadong massif was studied by the EPMA, M ssbauer spectroscopy, and Rietveld structural refinement using X-ray powder diffraction data. The ilmenite-bearing anorthosite shows complicated mineral assemblage which consists of plagioclase, clinopyroxene, hornblende, biotite, chlorite, apatite, allanite, and zircon. Anorthite is andesine in composition (Ab 28-57), and clinopyroxene drops in ferro-hypersthene (Fs 62-70). Ilmenite is trigonal symmetry with R space group, whose structure shows the alternation of Fe2+ (M1 site) octahedral layer and Ti (M2 site) layer along c axis. M ssbauer spectroscopy indicates that there are three doubles which assigned to couple of Fe2+($\delta$=0.812, 0.890mm/sec) and one Fe3+($\delta$=0.303mm/sec) in octahedral sites. Their Fe3+/$\Sigma$Fe is 0.065 and chemical formula is established as Fe2+0.94Fe3+0.07Ti0.97O3 using both EPMA and M ssbauer analysis. Rietveld structural refinement reveals that site occupancies of Fe in M1 and Ti in M2 are 91.2% and 89.4%, respectively. This implies that Ti and Fe2+ are alternatively occupy M1 and M2 sites. In addition, smaller M2 site is more preferable to Fe3+ occupancy over M1.

• 한국결정성장학회지
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• 제7권2호
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• pp.244-252
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• 1997

$LiCO_3, Al_2O_3, Fe_2O_3$ 혼합물을 1620K에서 반응시켜 리튬전지의 음극재료로 응용이 가능한 스핀넬형 $LiAl_{2.5}/Fe_{2.5}O_8$를 합성하였다. XRD의 Rietveld 해석을 통하여 결정구조 해석을 하였다. 고용체의 공간군은 $P4_3$32(a=8.1293$\AA$)이고, 결정구조해석의 최종 Residual index는 약 5%정도이었다. 역 스핀넬구조에서 양이온 $Al^{3+}, Fe^{3+}$은 4-배위와 6-배위로 위치하고, $Li^+$은 4b, 12d의 6-배위자리에 존재하였다.

• The Korean Journal of Ceramics
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• 제5권4호
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• pp.341-347
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• 1999

An ambiguity on the correct room temperature structure of $Bi_5Ti_3FeO_{15}$ was resolved using a combined Rietveld refinement of neutron and X-ray diffraction. The structure of this compound has been reported to have a space group of F2mm (adopting 2-fold rotation symmetry along the c-axis) or A21am. However, our diffraction, study reveals that some reflections would violate F-centering and confirm that the belong to $A2_1$am. Out refinement with the space group of $A2_1$am converged at $R_p=6.85%, R_wp=9.23%$ and $\chi^2$=1.66 for an isotropic temperature model with 85 variables. The lattice constants are a=5.4677(1) $\AA$, b=5.4396(1) $\AA$, and c=41.2475(8)$\AA$. In structure, Ti/Fe atoms at the oxygen octahedral sites of the perovskite unit are completely disordered, resulting in that these atoms are transparent in neutron diffraction. The octahedra of the perovskite unit are relatively displaced along the a-axis against the Bi atoms, which contribute as a major component to the spontaneous polarization of $Bi_5Ti_3FeO_{15}$.

• 한국세라믹학회지
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• 제40권6호
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• pp.513-518
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• 2003

La/sub 2/3-x/Li/sub 3x/□/sub 1/3-2x/TiO₃ compounds with x=0.13 and 0.12 were prepared by slow cooling (x=0.13) and rapid quenching (x=0.12) into the liquid nitrogen after sintering at 1350℃ for 6 h. Their crystal structure has been determined by Rietveld refinement of both the powder neutron and X-ray diffraction data. From neutron diffraction data, we found that the main phase was not tetragonal (P4/mmm), but trigonal (R3cH). The refinement of neutron diffraction for the slow cooled samples were in a good agreement with a new model; a mixture of trigonal (R3cH, 45.7 wt％), tetragonal (p4/mmm, 37.0 wt％), and Li/sub 0.57/Ti/sub 0.86/O₂(pbnm, 17.2 wt%), but the quenched sample was found not to contain tetragonal (p4/mmm). X-ray diffraction data couldn't be well fitted because of the Poor scattering factor of lithium ions and the similar reflection patterns among trigonal (R3cH), tetragonal (p4/mmm), and cubic (Pm3m). We also knew that one transport bottlenecks is destroyed by one La vacancy in the case of trigonal (R3cH).

• Progress in Superconductivity
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• 제13권3호
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• pp.178-183
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• 2012

Two $RuSr_2(EuCe)Cu_2O_z$ samples (as prepared and after $N_2$ treatment) have been investigated by thermogravimetric (TC) analysis, high-resolution x-ray powder diffraction and magnetization measurements. TG measurements which were carried out in $H_2/Ar$ atmosphere showed that the $N_2$ treatment of the as-prepared sample at $650^{\circ}C$ for 2h leads to a decrease in the oxygen content z by about 0.25. This oxygen depletion was accompanied by an increase in the magnetic transition temperature from 54.0 K to 114.9 K. This magnetic behavior is discussed in connection with the results of Rietveld analysis of the x-ray diffraction data which showed that the $N_2$ treatment resulted in both a significant increase in the rotation angle of the $RuO_6$ octahedra and a decrease in c-lattice parameter of the sample.

• 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.

• Progress in Superconductivity
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• 제1권2호
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• pp.135-140
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• 2000

Distribution of Pr ions between Y- and Ba-site of the $Y(Ba_{1-Xn}Pr_{Xn})_2Cu_3O_y$ ($0{\leq}Xn{\leq}{0.3}$, Xn : nominal composition) material prepared by the solid state reaction method was studied. Although the samples have narrow superconducting transition, tiny peaks of $Y_2BaCuO_5$ impurity phase are included in the x-ray diffraction patterns suggesting that some of the Pr ions are entered into the Y-site. The distribution of Pr ions between Y- and Ba-site was determined by measuring the mass fraction of YBCO and $Y_2BaCuO_5$ phase for each sample through the Rietveld analysis of the x-ray diffraction data. About 60 % of Pr ions occupy the Y-site regardless of the Pr content. Various superconducting parameters such as the oxygen content and the hole concentration etc. are compared before and after the impurity correction.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 1999년도 춘계학술대회 논문집
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• pp.337-340
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• 1999

Since the first reports of CMR(colossal magnetoresistance) effects in some single crystal R-P Phase Ln$_{1-x}$ Sr$_{2-x}$Mn$_{2}$O$_{7}$ 1996. many researches have been carried out to find optimum compositions and processing conditions in this system. In this study, layered perovskite R-P Phase Ln$_{1-x}$ Sr$_{2-x}$Mn$_{2}$O$_{7}$ (x=0.4, Ln=-La, Eu, Gd, Nd, Pr, Sm) phases were synthesized by solid state reaction and their structures were refined by Rietveld method. Electrical and magnetic properties were measured drown to 20K and compare with those of R-P Phase Ln$_{1-x}$ Sr$_{2-x}$Mn$_{2}$O$_{7}$ Phases.es.es.es.es.es.