• Title/Summary/Keyword: Rietveld analysis

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Neutron Diffraction Study of Powders Prepared by Self-propagating High Temperature Synthesis

  • Park, Yong;Kim, Y S.;Y. D. Hahn;S. H. Shim;Lee, J. S.
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2000.11a
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    • pp.11-12
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    • 2000
  • Non-stoichiometric ceramics of $Ni_{x}ZnO_{1-x}Fe_{2}O_{4}$ were prepared by self-propagating high temperature synthesis reaction with various processing conditions and their stoichometric numbers were determined by neutron diffraction. The neutron diffraction patterns were measured at room temperature using monochromatic neutrons with a wave length of 0.18339 nm from a Ge(331) mocochromator at a 90 degree take off angle. The Rietveld refinement of each pattern converged to good agreement (x2=1.88-2.24). The neutron diffraction analysis revealed the final stoichiometries of the ferrites were $Ni_{0.38}Zn_{0.62}Fe_{2}O_{4}$ and $Ni_{0.33}Zn_{0.67}Fe_{2}O_{4]$, respectively. This supports that final stoichiometric number of the self-propagating high temperature synthesis product can be controlled by the processing parameters during the combustion reaction.

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A Study on the S-block Structure in Hexagonal Ferrites (육방정 페라이트의 S-block 구조에 대한 연구)

  • 신형섭;이종협;권순주
    • Journal of the Korean Ceramic Society
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    • v.31 no.1
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    • pp.62-68
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    • 1994
  • It is compared the structures of the S-block in the Ba-Co-Zn Y-type hexagonal ferrites (Ba2Co2-xZnxFe12O22, x=0~2) and the Co-Zn spinel ferrites (Co1-xZnxFe2O4, x=0~1) expressed by a hexagonal axis system (space group R3m). The structures have been refined with a Rietveld analysis of the powder X-ray diffraction pattern with high precision (Rwp<0.13, RI<0.03). The overal dimension of the S-block is slightly different from the 1/3 of a hexagonal spinel unit cell as follow: 1.6~2.0% longer c-axis, 1.3~1.6% shorter a-axis and about 1% smaller volume. Upto Zn:Co=1:1 in the Ba-Co-Zn Y-type hexagonal ferrites, the zinc substitute primarily the tetrahedral sites in the S-block. Beyond that the zinc seems to go into the T-block as well.

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Quantitative Analysis of Hydrate of Sugar-based Super Retardign Agent Mixed Cement Paste Using Rietveld Method (리트벨트법을 이용한 당류계 초지연성 혼화제 혼입 시멘트 페이스트의 수화생성물 정량 분석)

  • Hyun, Seung-Yong;Hu, Yun-yao;Kim, Su-Hoo;Kim, Jong;Han, Min-Cheol;Han, Cheon-Goo
    • Proceedings of the Korean Institute of Building Construction Conference
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    • 2021.11a
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    • pp.74-75
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    • 2021
  • This study attempted to study the setting time and compressive strength according to the sugar type through XRD. Setting time was found to be delayed the most when mixing white sugar, and setting time was promoted when mixing Saccharin and Aspartame. It was found that when white sugar and Grosvener siraitia were mixed, the compressive strength was higher than that of Control. Aspartame the age passed, C3S decreased and Ca(OH)2 increased.

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${29}^Si$ MAS NMR Study on Quantitative Analysis of the Amorphous Phase in a $Si_3N_4$ Powder

  • Fujimori, Hirotaka;Kitahara, Hiromoto;Ioku, Koji;Goto, Seishi;Nakayasu, Tetsuo;Yamada, Tetsuo
    • The Korean Journal of Ceramics
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    • v.6 no.2
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    • pp.155-158
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    • 2000
  • NMR study has been used for measuring precise quantity of the amorphous phase in the $Si_3N_4$powder. Care must be taken to allow the $^{29}$Si nuclear spin system to fully relax between pulses in order to make the signals proportional to the number of nuclei in each phase. $^{29}$Si MAS spectrum was decomposed into the three spectra of $\alpha$-, $\beta$-, and amorphous $Si_3N_4$assuming pseudo-Voigt function. Moreover, the Rietveld analysis of the powder X-ray diffraction data was performed to measure quantity of crystalline phases as $\alpha/\beta$ ratio.

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Thermal Properties of 0.9CaMgSi2O6-0.1MgSiO3 Glass-Ceramics

  • Jeon, Chang-Jun;Sun, Gui-Nam;Lee, Jong-Kyu;Ju, Han-Sae;Kim, Eung-Soo
    • Journal of the Korean Ceramic Society
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    • v.49 no.1
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    • pp.111-117
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    • 2012
  • Dependencies of thermal properties on the crystallization behavior of $0.9CaMgSi_2O_6-0.1MgSiO_3$ glass-ceramics were investigated as a function of heat-treatment temperature from $750^{\circ}C$ to $950^{\circ}C$. The crystallization behavior of the specimens depended on the heat-treatment temperature, which could be evaluated by differential thermal analysis (DTA), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction (XRD) analysis by the Rietveld-reference intensity ratio (RIR) combined procedure. With an increase of the heat-treatment temperature, the thermal conductivity and thermal diffusivity of the heat-treated specimens increased. These results could be attributed to the increase of crystallization with heat-treatment temperature. However, the specific heat capacity of the heat-treated specimens was not affected by the heat-treatment temperature. The thermal conductivities measured from $25^{\circ}C$ to $100^{\circ}C$ were also discussed for application to lighting-emitting diode (LED) packages and substrate materials.

Exploration of structural, thermal and spectroscopic properties of self-activated sulfate Eu2(SO4)3 with isolated SO4 groups

  • Denisenko, Yu.G.;Aleksandrovsky, A.S.;Atuchin, V.V.;Krylov, A.S.;Molokeev, M.S.;Oreshonkov, A.S.;Shestakov, N.P.;Andreev, O.V.
    • Journal of Industrial and Engineering Chemistry
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    • v.68
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    • pp.109-116
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    • 2018
  • $Eu_2(SO_4)_3$ was synthesized by chemical precipitation method and the crystal structure was determined by Rietveld analysis. The compound crystallizes in monoclinic space group C2/c. In the air environment, $Eu_2(SO_4)_3$ is stable up to $670^{\circ}C$. The sample of $Eu_2(SO_4)_3$ was examined by Raman, Fourier-transform infrared absorption and luminescence spectroscopy methods. The low site symmetry of $SO_4$ tetrahedra results in the appearance of the IR inactive ${\nu}_1$ mode around $1000cm^{-1}$ and ${\nu}_2$ modes below $500cm^{-1}$. The band intensities redistribution in the luminescent spectra of $Eu^{3+}$ ions is analyzed in terms of the peculiarities of its local environment.

USE OF NEAR INFRARED FOR THE QUANTITATIVE ANALYSES OF BAUXITE

  • Walker, Graham S.;Cirulis, Robyn;Fletcher, Benjimin;Chandrashekar, S.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1171-1171
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    • 2001
  • Quantitative analysis is an important requirement in exploration, mining and processing of minerals. There is an increasing need for the use of quantitative mineralogical data to assist with bore hole logging, deposit delineation, grade control, feed to processing plants and monitoring of solid process residues. Quantitative analysis using X-Ray Powder Diffraction (XRD) requires fine grinding and the addition of a reference material, or the application of Rietveld analysis to XRD patterns to provide accurate analysis of the suite of minerals present. Whilst accurate quantitative data can be obtained in this manner, the method is time consuming and limited to the laboratory. Mid infrared when combined with multivariant analysis has also been used for quantitative analysis. However, factors such as the absorption coefficients and refractive index of the minerals requires special sample preparation and dilution in a dispersive medium, such as KBr to minimize distortion of spectral features. In contrast, the lower intensity of the overtones and combinations of the fundamental vibrations in the near infrared allow direct measurement of virtually any solid without special sample preparation or dilution. Thus Near Infrared Spectroscopy (NIR) has found application for quantitative on-line/in line analysis and control in a range of processing applications which include, moisture control in clay and textile processing, fermentation processes, wheat analysis, gasoline analysis and chemicals and polymers. It is developing rapidly in the mineral exploration industry and has been underpinned by the development of portable NIR spectrometers and spectral libraries of a wide range of minerals. For example, iron ores have been identified and characterized in terms of the individual mineral components using field spectrometers. Data acquisition time of NIR field instruments is of the order of seconds and sample preparation is minimal. Consequently these types of spectrometers have great potential for in-line or on-line application in the minerals industry. To demonstrate the applicability of NIR field spectroscopy for quantitative analysis of minerals, a specific example on the quantification of lateritic bauxites will be presented. It has been shown that the application of Partial Least Squares regression analysis (PLS) to the NIR spectra can be used to quantify chemistry and mineralogy in a range of lateritic bauxites. Important, issues such as sampling, precision, repeatability, and replication which influence the results will be discussed.

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Mineral Compositions of Korean Dancheong Pigment Products using Quantitative XRD (정량 X-선 회절분석을 이용한 국내시판 단청안료의 광물조성 연구)

  • Moon, Dong Hyeok;Han, Min Su;Jeong, Hye Young;Go, In Hee;Cho, Hyen Goo
    • Journal of Conservation Science
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    • v.32 no.3
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    • pp.403-416
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    • 2016
  • Mineral composition and content of 22 Korean Dancheong pigment products were obtained by Rietveld quantitative analysis. Jubosa, Hwang, Seokrok, Seokcheong and Hobun consist of pure cinnabar, orpiment, malachite, azurite and calcite (or aragonite), respectively. Whereas Seokganju, Hwangto, Noerok, Lapis lazuli, Baekto and Cockie hobun mainly consist of hematite, goethite, celadonite, lazurite, kaolin mineral and portlandite, respectively. And they all consist of soil minerals (quartz, feldspar, sericite and vermiculite) and filler minerals in the industry field (calcite, gypsum and anhydrite) at a different content. Quantitative XRD proved more useful method to determined exact mineral composition and content than chemical or microscopical data. If this method utilize for specification of natural pigment product, it is considered to be applicable in restoration technology and conservation science field.

Phase transition and crystal structure analysis of PTCR $BaTiO_3$ ceramics with dopants (Y, Nb) (첨가제(Y, Nb)에 따른 PTCR $BaTiO_3$계 세라믹스의 결정구조 해석과 상전이 특성)

  • 차용원;원승신;백종후;이희수;엄우식;송준광;이인식;정훈택
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.2
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    • pp.253-258
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    • 1997
  • The characteristics of crystal structure and phase transition with dopants ($Nb_2O_5$= 0.1~0.4 mol% and $Y_2O_3$ : 0.2~0.4 mol%) on the PTCR $BaTiO_3$ system were investigated. In the case of $Nb_2O_5$ additive, the lattice parameter of PTCR $BaTiO_3$ was changed linearly with the increasement of $Nb_2O_5$ which substituted B-site of BaTiO$_3$ and the lattice parameter of c-axis decreased abruptly at 0.3 mol%. These phenonmena were assumed to originate from the distortion of octahedron and we could confirm that the change of lattice parameter accorded with the characteristics of the phase transition temperature. $Y^{3+}$ ions substituted both of A- and B-site until the 0.3 mol% addition, but $Y^{3+}$ substitution preferred A- to B-site above 0.3 mol%. This was affirmed by the variation ,of lattice parameter and the characteristics of phase transition. It also was found that $Y^{3+}$ions in the A-site substituted both of $Ba^{2+}$ and $Ca^{2+}$ ions with equal ratio by Rietveld method.

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Analysis of the Crystal Structure and the Relation with the Temperature Coefficient au_\varepsilon$ in $BaORe_2O_3TiO_2$ (Re=La, Nd, Y) Microwave Dielectric Ceramics ($BaORe_2O_3TiO_2$ (Re=La, Nd, Y)계 고주파 유전체의 결정구조 분석 및 온도계수 au_\varepsilon$와의 관련성)

  • 김정석;강현주;심해섭;이창희;천채일
    • Journal of the Korean Ceramic Society
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    • v.36 no.2
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    • pp.136-144
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    • 1999
  • Crystal structures of tungsten-bronze type microwave dielectric ceramics, $BaOLa_2O_34TiO_2$ (BLT) and $BaO(Nd_{0.77}Y_{0.23})_4TiO_2$ (B(NY)T), were analysed using the Rietveld method. The most relibale refinement was obtained by refining the cation and anion positions from the x-ray and neutron diffraction data, respectively. The ambiguites inherent in the refined crystal structure by Mateeva et al. were resolved. The $BaORe_2O_34TiO_2$ structure consiste of $3\times2$ perovskite blocks and 4 pentagon-channels. The Ti-O6 octahedrons are distroted and tilted, which, consequently, induces the displacements of Ba and Re ions producing the superlattics (c$\approx$ 7.6 $\AA$). The B(NY)T showed more severely tilted Ti-O6 octahedrons. The relative dielectric constant $\varepsilon_{\gamma}$ and temperature coefficient $\tau_\varepsilon$ are 109.5 and-$180 ppm/^{\circ}C$ in BLT, 76 and $+40 ppm/^{\circ}C$ in B(NY)T, respectively. The small Re ions produced a positive $\tau_\varepsilon$. The relation between $\tau_\varepsilon$ and the octahedron tilting in complex perovskite is discussed for the tungsten bronze type structure.

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