• Title/Summary/Keyword: Quantitative XRD

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Quantitative Analysis of Feldspar Mixture Samples Using the Rietveld Refinement Method (Rietveld Refinement 방법을 응용한 장석 혼합시료의 정량분석 연구)

  • Shim, Sang-Heon;Ahn, Jung-Ho;Kim, Soo-Jin
    • Journal of the Mineralogical Society of Korea
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    • v.7 no.1
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    • pp.62-79
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    • 1994
  • The quanttative and structural analysis of the binary standard mixtures of albite and quartz, and microcline and albite were carried out using the Rietveld refinement method in order to investigate the accuracy and precision of the method. The quantitative analysis using the Rietveld method results in a standard deviation of 4 wt % for the albite-quartz standard mixtures and 1 wt % for the microcline-albite standard mixtures, suggesting that its accuracy is far better than that of the conventional XRD method in which only a few selected peaks are utilized. Furthermore, the unit-cell parameters of component minerals in mixtures were also estimated accurately during the analysis. It was observed that the refined weight fractions deviate systematically from their measured values when the method is applied to the mixtures that contain minerals with different degrees of preferred orientation, such as albite-quartz mixtures. The preferred orientation parameters and R-values suggest that the systematic deviation is caused as a result of the preferred orientation effect of feldspar crystallites. It is evident that the preferred orientation corrections are of help for the accurate determination of unit-cell parameters, although they may not improve the result of quantitative analysis significantly. The refined weight fraction of the mineral with higher degree of preferred orientation in mixture is greater than the measured one. This is apparently caused by the effect of geometry of feldspar crystallites in the surface of the mounted sample. The Rietveld refinement method minimizes the problems inherent in the traditional XRD methods, such as the line overlap, primary extinction, and preferred orientation effect, by fitting every data point in a whole pattern explicitly. Furthermore, accurate unit-cell parameters as well as scale factors that can be obtained from the Rietveld refinement are used for the quqantification. The present stdudy demonstrates that the Rietveld method yields far more accurate analytical result than the conventional XRD quantitative analysis method does.

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Study on the Effect of Fineness and Substitution Rate of Natural Zeolites on Chemical Reaction and Physical Properties of Cement Mortar (천연 제올라이트의 분말도와 치환율이 시멘트모르타르의 화학반응 및 물리적 특성에 미치는 영향에 관한 연구)

  • Yoon, Chang-Bok;Lee, Han-Seung
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.24 no.3
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    • pp.96-103
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    • 2020
  • As a basic study for the application of natural zeolite as a concrete admixture, the compressive strength, activity factor, Ca(OH)2 quantitative analysis and XRD experiments were investigated. It is thought that SiO2, which is abundant in natural zeolite, affects the strength development by reacting with the hydration product of cement in all specimens in which natural zeolite was added according to powder level and substitution rate. As the substitution rate increases, the compressive strength decreases, which is considered to be due to the decrease in the amount of C3S and C2S minerals in the clinker, which affects the strength expression compared to the cement content of the reference mortar. The XRD crystal structure did not show a significant difference from the reference mortar, and it was confirmed that the Z2-10 (Blaine: 15,600㎠ / g) specimen with 10% substitution of natural zeolite was the best among the experimental levels. Substitution amount for use as concrete admixture is 10% substitution is most ideally seen.

A Study on the Quantitative Analysis of Crystalline Phase Cordierite Composition (코디어라이트 조성에 있어서 결정질 상의 정량분석에 관한 연구)

  • 박용완;현부성;원종원
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.3 no.2
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    • pp.157-161
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    • 1993
  • 결정화 유리에서의 결정질 양의 측정, 혹은 소결체에서의 잔류 유리량을 측정할 때 유용한 방법을 찾아내기 위하여 현재까지 보고되어 있는 방법중에서 XRD를 이용한 Ohlberg의 방법과 Wakelin등의 방법을 이용하여 코디어라이트 조성의 유리와 α-코디어라이트의 혼합물에 대하여 결정질 양을 측정하였다. Ohlberg의 방법은 한 각도에서 측정하는 경우, 약 4∼5%의 오차를, 4각도에서 측정하여 평균한 경우에는 2∼3%의 오차를 보였으며, Wakelin등의 방법은 실험 양이 많았지만 2∼3%의 오차를 보였다.

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The various bonding structure of SiOC thin films attributed to the carbon density (탄소밀도의 변화가 SiOC 박막의 결합구조에 미치는 영향)

  • Oh Teresa
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.43 no.5 s.347
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    • pp.11-16
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    • 2006
  • This paper reports the correlation between dielectric constant and degree of amorphism of the hybrid type SiOC thin films. SiOC thin films were deposited by high density plasma chemical vapor deposition using bistrimethyl- silylmethane(BTMSM,$H_{9}C_{3}-Si-CH_{2}-Si-C_{3}H_{9}$) and oxygen precursors with various flow rate ratio. As-deposited film and annealed films at $400^{\circ}C$ were analyzed by XRD. The SiOC thin films were amorphous from XRD patterns. For quantitative analysis, the diffraction pattern of the samples was transformed to radial distribution function by Fourier analysis, and then compared with each other. The degree of amorphism of annealed films was higher than that of as-deposited ones. The dielectric constant varied in accordance with flow rate ratio of precursors. The lowest dielectric constant was obtained from the as-deposited film which has the highest degree of amorphism after annealing.

Characterization of crystal phase evolution in cordierite honeycomb for diesel particulate filter by using rietveld refinement and SEM-EDS methods (Rietveld 정밀화법과 SEM-EDS 분석에 의한 DPF용 코디어라이트 하니컴 세라믹스의 결정성장 과정 분석)

  • Chae, Ki-Woong;Kim, Kang San;Kim, Jeong Seog;Kim, Shin-Han
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.3
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    • pp.116-126
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    • 2021
  • Diesel particulate filter (DPF) is a typical application field of cordierite (Mg2Al4Si5O18) honeycomb. Green body for DPF honeycomb was extruded using slurry paste and sintered at the temperature range of 980~1450℃. Quantitative crystal phase analysis was carried out by using Rietveld refinement method for powder XRD data. In conjunction with the quantitative Rietveld analysis, SEM-EDS analysis was carried for the crystal phases (indialite, cordierite, cristobalite, alumina, spinel, mullite, pro-enstatite). After removing amorphous phase on the sintered surfaces by chemical etching method, the shape and composition of the crystal phases can be clearly identified by SEM-EDS method. By combining the Rietveld refinement method and SEM-EDS analysis, crystal phase evolution process in DPF cordierite ceramics could be clarified. In addition, the coefficient of thermal expansion (CTE) of the DPF honeycombs were measured and compared with the calculated CTEs based on the quantitative crystal phase analysis results.

TEM Specimen Preparation Method of Gibbsite Powder for Quantitative Structure Analysis (정량 구조 분석을 위한 Gibbsite 분말의 TEM 시편 준비법)

  • Kim, Young-Min;Jeung, Jong-Man;Lee, Su-Jeong;Kim, Youn-Joong
    • Applied Microscopy
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    • v.32 no.4
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    • pp.311-317
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    • 2002
  • There is great requirement on the TEM specimen preparation method with particle size selectivity as a prerequisite for the quantitative structure analysis on the materials such as gibbsite powder, which generally forms a large agglomerate and shows a variation of transition process depending on their sizes. In this experiment, we made an attempt to give a methodology for the TEM specimen preparation of powder with the size selectivity. After mixing 1 wt% gibbsite powder with ethanol solvent, gibbsite suspension was prepared by application of ball-milling and ultrasonification with addition of 0.25 vol% dispersion agent, Darvan C, which was diluted into distilled water by the ratio 1:19. Appling the static sedimentation method to gibbsite suspension after estimation of the sedimentation time by the measurement of accumulative concentration variation, we acquired TEM specimens with well-dispersed and size selected gibbsite particles in nm scale. Overall picture of each sample was taken by SEM and morphology of each dispersed particle was imaged by TEM. Raw and processed gibbsite powders were also examined by XRD to investigate whether they were suffered from phase change during the process or not.

Densification and Dielectric Properties of Ba0.5Sr0.5TiO3-Glass Composites for LTCC Applications

  • Shin, Hyun-Ho;Byun, Tae-Hun;Yoon, Sang-Ok
    • Journal of the Korean Ceramic Society
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    • v.49 no.1
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    • pp.100-104
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    • 2012
  • Barium zincoborate (BZB) glass was added to $Ba_{0.5}Sr_{0.5}TiO_3$, and sintered at $875^{\circ}C$ for 2 h in air. When the BZB glass was added in quantities ranging from 15 to 20 wt%, the relative bulk density ranged from 93.1% to 94.2%, while the density decreased to roughly 81% thereafter up to 30 wt% glass addition. Quantitative XRD analysis showed that the $Ba_{0.5}Sr_{0.5}TiO_3$ filler was significantly dissolved into the BZB glass. However, no secondary phase was identified by XRD up to 30 wt% glass addition. The dielectric constant was about 130 to 140 at 1MHz up to 20 wt% BZB glass addition, while it decreased to about 60 thereafter, which may be ascribed to decreased density, partial dissolution of the $Ba_{0.5}Sr_{0.5}TiO_3$, and associated changes in the glass composition. The dielectric loss of the 20 wt% glass added specimen was 0.008.

Crystal Structure and Quantitative Phase Analysis of Multiphase Sample using RIETAN and MEED (RIETAN 및 MEED법에 의한 다상시료의 결정구조 및 정량상 분석)

  • 김광복;천희곤;조동율;신종근;구경완
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.07a
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    • pp.303-307
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    • 2000
  • The crystal structure of ZnS fabricated by gas-liquid phase reaction was obtained by XRD and refined by RIETAN near R$_{wp}$ factor 10%. The increasement of HCP phase depended on extra H$_2$S gas and the lattice parameter and crystalline size changed by the relative ratio of multiphase. Using ZnS of the different multiphase ratio and crystalline size, sintered ZnS:Cu, Al green phosphor and the CL property resulted optimum luminescence in the range of 91~94% and 150~190$\AA$, respectably, FCC/HCP ratio and crystalline size. As changing of structure ratio, the reason of different luminescence property is now studying. As well as, after XRD pattern of TiO$_2$powder fitted by RIETAN and the structure factor using MEED method simulated about each atom of (002) plane. Additionally, we proposed RIETAN and MEED were the methods of the study of luminescence mechanism for many phosphor materials.s.

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The study of detonation of laser-ablated aluminum by high power laser (고 에너지 레이저를 통한 laser-ablated 알루미늄의 detonation 현상 연구)

  • Kim, Chang-Hwan;Yoh, Jack. J
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2011.04a
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    • pp.425-429
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    • 2011
  • The development of metal plasma generated by high laser irradiance and its effect on the surrounding air using shadowgraph images after laser pulse termination are studied; hence the formation of laser supported detonation and combustion processes has been investigated. The core of the paper is in detecting chemical reaction using X-Ray Diffraction (XRD) between ablated aluminum plasma and oxygen from air by inducing high power laser pulse (>1000 mJ/pulse) and conduct a quantitative comparison of chemically reactive laser initiated waves with the classical detonation of exploding aluminum (dust) cloud in air. This study may suggest a new approach of initiating detonation from metal sample in its bulk form without the need of mixing nano-particles with oxygen for initiation.

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Nb-carbonitride Analysis Techniques in Nb-steels (강 중 Nb계 탄질화 석출물 정량분석 기술)

  • Lee, J.J.;Jung, S.W.;Yoo, K.S.
    • Analytical Science and Technology
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    • v.7 no.4
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    • pp.493-504
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    • 1994
  • The morphology and structure of precipitates of formed in Nb steels were investigated using SEM, TEM and XRD. The quantitative analysis of the precipitates was performed by ICP-AES. The potentiostatic etching method was employed as an extraction method using 10% AA-methanol and 15% Na-citrate electrolytes. The two selected potentials relative to SCE(Standard Calomel Electrode), -100mV in 10% AA-methanol solution and -250mV in 15% Na-citrate solution were found to be effective for the extraction. XRD analysis showed that composition of Nb carbonitride in Nb-steel(0.01% C-0.7% Nb-0.004N) was $NbC_{0.65}N_{0.2}$.

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