• 제목/요약/키워드: Rietveld Analysis

검색결과 84건 처리시간 0.026초

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.
    • 한국분말야금학회:학술대회논문집
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    • 한국분말야금학회 2000년도 추계학술대회 및 발표대회 강연 및 발표논문 초록집
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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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육방정 페라이트의 S-block 구조에 대한 연구 (A Study on the S-block Structure in Hexagonal Ferrites)

  • 신형섭;이종협;권순주
    • 한국세라믹학회지
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    • 제31권1호
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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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리트벨트법을 이용한 당류계 초지연성 혼화제 혼입 시멘트 페이스트의 수화생성물 정량 분석 (Quantitative Analysis of Hydrate of Sugar-based Super Retardign Agent Mixed Cement Paste Using Rietveld Method)

  • 현승용;후윈야오;김수호;김종;한민철;한천구
    • 한국건축시공학회:학술대회논문집
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    • 한국건축시공학회 2021년도 가을 학술논문 발표대회
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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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    • 제6권2호
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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
    • 한국세라믹학회지
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    • 제49권1호
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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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    • 제68권
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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.
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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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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정량 X-선 회절분석을 이용한 국내시판 단청안료의 광물조성 연구 (Mineral Compositions of Korean Dancheong Pigment Products using Quantitative XRD)

  • 문동혁;한민수;정혜영;고인희;조현구
    • 보존과학회지
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    • 제32권3호
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    • pp.403-416
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    • 2016
  • 본 연구는 현재 단청시공에 실제 사용되고 있는 국산 천연안료 제품 총 22종을 대상으로 리트벨트법을 활용한 정량 X-선 회절분석을 실시하여 구성성분의 조성과 함량 특성을 밝히고자 하였다. 분석결과, 주보사와 황, 석록, 석청, 호분 등의 제품들은 각각 거의 순수한 진사, 웅황, 공작석, 남동석 및 방해석 또는 아라고나이트로 구성된 것으로 판단된다. 반면, 석간주와 황토, 뇌록, 라피스라즐리, 백토, 꼬막호분 등의 제품들은 각각 적철석, 침철석, 뇌록석, 라주라이트, 고령석 및 포틀랜드석 등이 주구성광물이며, 그 외 석영, 장석, 견운모, 질석 등 일반적인 토양에 풍부한 광물과 방해석, 석고 및 경석고 등과 같이 산업계에서 충진제로 활용되는 광물들이 각 제품에 다양한 비율로 함유되어 있는 것으로 나타났다. 이와 같이 정량 X-선 회절분석을 통하여 화학조성분석이나 현미경관찰만으로는 획득하기 쉽지 않은 보다 구체적인 안료 제품들의 광물조성 및 그 함량 비에 대한 정보를 획득할 수 있었으며, 추후 이를 천연안료제품의 품질기준 설정에 활용하거나 대체원료수급 및 품질향상을 통한 보존과학연구 등에 다양한 방법으로 적용이 가능할 것으로 사료된다.

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

  • 차용원;원승신;백종후;이희수;엄우식;송준광;이인식;정훈택
    • 한국결정성장학회지
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    • 제7권2호
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    • pp.253-258
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    • 1997
  • 반도체화 첨가제인 $Y_2O_3$$Nb_2O_5$ 첨가랑 변화에 따른 PTCR $BaTiO_3$ 세라믹스의 결정구조 해석과 상전이 특성을 연구하기 위하여 ($Ba_{0.85}Ca_{0.15})TiO_3$ + X m/o $Nb_2O_5$(Y m/o $Y_2O_3$) + 0.08 w/o $Mn(NO_3)_2$$6H_2O$ + 0.25 w/o $SiO_2$ 계에서 X는 0.1 ~ 0.4로 Y는 0.2 ~ 0.4로 각각 변화시켜 실험을 수행하였다. $Nb_2O_5$의 첨가시 B-site 치환에 따라서 격자상수가 선형적으로 변화하다가 0.3 mol% 이상 치환할 경우 c 축의 격자상수가 급격히 감소함을 알 수 있었다. 이는 octahedron distortion둥의 원인으로 판단되며, 이러한 격자상수 변화는 상전이 온도 결과와도 잘 일치함을 확인할 수 있었다. 또한 $Y_2O_3$ 첨가의 경우 0.3 mol%가지는 A, B-site를 각각 치환하며 그 이상부터는 A-site 이온을 주로 치환하는 것을 격자상수 변화와 상전이 온도결과를 통해 알 수 있었으며, Rietveld 해석결과 $Y^{3+}$가 A-site 치환시 $Ba^{2+}$$Ca^{2+}$를 같은 비율로 치환한다는 것을 알 수 있었다.

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

  • 김정석;강현주;심해섭;이창희;천채일
    • 한국세라믹학회지
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    • 제36권2호
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    • pp.136-144
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    • 1999
  • 텅스템브론즈형 고주파 유전체의 $BaORe_2O_3TiO_2$(BLT)와 $BaO(Nd({0.77}Y_{0.23})_2O_34TiO_2(B(NY)T)$의 결정구조를 Rietveld 정밀화법으로 분석하였다. 양이온은 X-선 데이터로부터, 산소이온은 중성자 데이터로부터 정밀화한 'combined법'에 의해 가장 신뢰성이 높은 결정구조분석 결과를 얻었다. Mateeva 등이 처음 제시한 결정구조의 결정학적 모순점을 해결하였다. BaORe2O34TiO2(Re=La, Nd, Y) 유전체는 $3\times2$개의 페롭스카이트 블록과 이 블록사이에 형성된 4개의 pentagon-channel로 이뤄진다. Ti-O6팔면체는 tilted 및 변형된 구조를 갖고 있고, 이에 의해 같은 z-층에 있는 Ba 및 Re 이온의 변위되어 초격자(c$\approx$ 7.6$\AA$)를 형성된다. Re 이온반경이 작은 B(NY)T의 Ti-O6 팔면체가 tilting 및 변형이 큰 것으로 나타났다. 유전상수 $\varepsilon_{\gamma}$과 온도계수 $au_\varepsilon$은 BLT의 경우 각각 $109.5, -180 ppm/^{\circ}C$였고, B(NY)T 경우 $76, +40ppm/^{\circ}C$이었다. Re 이온 크기가 작은 시료의 $\tau$$\varepsilon$이 +값을 나타내었다. 복합 페롭스카이트에서 관찰되는 $\tau_\varepsilon$과 팔면체 tilting과의 관계를 본 텅스텐 브론즈 구조재료에서 고찰하였다.

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