• Title/Summary/Keyword: X-ray diffraction(XRD)

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The analytical application for cement using X-Ray diffraction and X-Ray fluorescence spectrometer (X-Ray Diffraction과 X-Ray Fluorescence를 이용한 시멘트 비교 분석)

  • Jung, Ji Eun;Jang, Yu Rim;Kim, Ki-Wook;Heo, Sangcheol;Min, Ji-Sook
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.340-351
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    • 2013
  • The chemical element and structural characterization of different types of cements and its brick stones are been investigated under forensic aspects using X-ray florescence (XRF) and X-ray diffraction (XRD) spectrometer. The XRF provides rapid compositional data for controlling almost all stages of raw materials, clinker and cement. The decisive advantage of XRD methods is based on the unique character of the diffraction patterns of crystalline substances, the ability to distinguish between elements and their oxides, and the possibility to identify chemical compounds, polymeric forms, and mixed crystals by non-destructive examination. Therefore, combination of these examinations is useful and able to apply for the forensic analysis in comparison of cements and brick stones. There are more study remained to determine the viability of method for forensic analysis of brick stones and the limits of the discrimination that can be achieved.

X-ray Diffraction Analysis of Residual Stress in Laminated Ceramic

  • Jin, Young-Ho;Chung, Dong-Yoon
    • Journal of the Korean Ceramic Society
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    • v.48 no.5
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    • pp.458-462
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    • 2011
  • The strength of ceramic was improved by lamination by suppressing the propagation of cracks with compressive residual stress in the face layer of the laminate. Hot pressed SiAlON+SiC/SiC/SiAlON+SiC laminate discs were fabricated for tailored residual stress. The residual stress in this laminate was studied by X-ray diffraction (XRD). There was considerable compressive residual stress in the face layer. A Finite Element Analysis (FEA) was performed to support the measured XRD results and to determine the stress field in the laminate. The residual stress measured by XRD had satisfactory agreement with the analytically calculated and FEA values. The measured value by XRD was -385 ${\pm}$ 20 MPa over most of the face layer. The calculated and FEA values were -386 MPa and -371MPa, respectively. FEA also showed significantly modified stresses and the maximum tensile stress near the edge region which are possible crack generators in the presence of flaws or contact damage.

A study of semi-quantification of the Friedel's salt using the X-ray diffraction method in concrete (콘크리트 내 Friedel염의 XRD를 이용한 반정량적 측정기법에 관한 연구)

  • Lee, Ho-Jae;Lee, Jang-Hwa;Kim, Do-Gyeum
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.33-38
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    • 2012
  • Despite the importance of chloride binding, it is very difficult to measure the binding capacity, in particular, for the concrete body in an existing structure: in fact, the measurement procedure for chloride binding is much influenced by the environmental condition such as temperature, fineness of sample and pore water extraction techniques. The present study concerns the quantification of the binding capacity of chloride ions in concrete using the X-ray diffraction (XRD) technique. Once the binding isotherm of chlorides was determined by the Langmuir isotherm, as a function of the W/C, curing age and binder type, the generation of bound chlorides (i.e. Friedel's salt) was simultaneously ensured by the XRD technique. The amount of bound chloride was then determined by analyzing the peak intensity for the bound chlorides in the XRD curve. It was found that an increase in the curing age and a decrease in the W/C resulted in an increase in the binding capacity.

Modification of conventional X-ray diffractometer for the measurement of phase distribution in a narrow region

  • Park, Yang-Soon;Han, Sun-Ho;Kim, Jong-Goo;Jee, Kwang-Yong;Kim, Won-Ho
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.407-414
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    • 2006
  • An X-ray diffractometer for spatially resolved X-ray diffraction measurements was developed to identify phase in the narrow (micron-scaled) region of high burn-up fuels and some nuclear materials. The micro-XRD was composed of an X-ray microbeam alignment system and a sample micro translation system instead of a normal slit and a fixed sample stage in a commercial XRD. The X-ray microbeam alignment system was fabricated with a microbeam concentrator having two Ni deposited mirrors, a vertical positioner, and a tilt table for the generation of a concentrated microbeam. The sample micro translation system was made with a sample holder and a horizontal translator, allowing movement of a specimen at $5{\mu}m$ steps. The angular intensity profile of the microbeam generated through a concentrator was symmetric and not distorted. The size of the microbeam was $4,000{\times}20{\mu}m$ and the spatial resolution of the beam was $47{\mu}m$ at the sample position. When the diffraction peaks were measured for a $UO_2$ pellet specimen by this system, the reproducibility ($2{\Theta}={\pm}0.01^{\circ}$) of the peaks was as good as a conventional X-ray diffractometer. For the cross section of oxidized titanium metal, not only $TiO_2$ in an outer layer but also TiO near an oxide-metal interface was observed.

Application of Quantitative X-ray Diffraction Analysis for Unburned Coal Content on Coke-Char-Sinter Mixtures (고온에서 발생한 코크스-미연소탄-소결광의 혼합물 중 미연소탄의 정량화를 위한 분말 X-선 회절법 적용)

  • 김재명;정진경;김성만;허완욱;김형순
    • Journal of the Korean Ceramic Society
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    • v.40 no.5
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    • pp.481-487
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    • 2003
  • A technique for determination of proportions of char, coal ana coke is needed in order to monitor pulverized coal injection performance in operating blast furnace. Quantitative X-ray powder diffraction analysis can be applied to the problem providing that structural information on carbonaceous materials, coal, char, coke and their mixture are known. Chars were prepared from a coal at different temperatures (1000∼1400$^{\circ}C$) and were characterised by X-Ray powder Diffraction (XRD). The XRD result gave crystallite size (height Lc and diameter, La), aromaticity, number of (002) plane in carbon, and d-spacing. As a result, with increasing heat treat temperature of char, Lc$_{(002)}$, La$_{(10)}$ and number of (002) plane in carbon were increased, and d-spacing and FWHM(Full With Half Maximum) were decreased. Result of prediction of amount of char from the mixtures (char, coke and ore) based on the Lc$_{(002)}$ information of two mixtures (coke and char) showed very close values expected.

In situ Electric-Field-Dependent X-Ray Diffraction Experiments for Ferroelectric Ceramics (강유전 세라믹의 전기장 인가에 따른 in situ X-선 회절 실험)

  • Choi, Jin San;Kim, Tae Heon;Ahn, Chang Won
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.35 no.5
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    • pp.431-438
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    • 2022
  • In functional materials, in situ experimental techniques as a function of external stimulus (e.g., electric field, magnetic field, light, etc.) or changes in ambient environments (e.g., temperature, humidity, pressure, etc.) are highly essential for analyzing how the physical properties of target materials are activated/evolved by the given stimulation. In particular, in situ electric-field-dependent X-ray diffraction (XRD) measurements have been extensively utilized for understanding the underlying mechanisms of the emerging electromechanical responses to external electric field in various ferroelectric, piezoelectric, and electrostrictive materials. This tutorial article briefly introduces basic principles/key concepts of in situ electric-field-dependent XRD analysis using a lab-scale XRD machine. We anticipate that the in situ XRD method provides a practical tool to systematically identify/monitor a structural modification of various electromechanical materials driven by applying an external electric field.

X-Ray Diffraction Analysis of Various Calcium Silicate-Based Materials

  • An, So-Youn;Lee, Myung-Jin;Shim, Youn-Soo
    • Journal of dental hygiene science
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    • v.22 no.3
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    • pp.191-198
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    • 2022
  • Background: The purpose of this study was to evaluate the composition of the crystal phases of various calcium silicate-based materials (CSMs): ProRoot white MTA (mineral trioxide aggregate) (WMTA), Ortho MTA (OM), Endocem MTA (EM), Retro MTA (RM), Endocem Zr (EN-Z), BiodentineTM (BD), EZ-sealTM (EZ), and OrthoMTA III (OM3). Methods: In a sample holder, 5 g of the powder sample was placed and the top surface of the material was packed flat using a sterilized glass slide. The prepared slides were mounted on an X-ray diffraction (XRD) instrument (D8 Advance; Bruker AXS GmbH, Germany). The X-ray beam 2θ angle range was set at 10~90° and scanned at 1.2° per minute. The Cu X-ray source set to operate at 40 kV and 40 mA in the continuous mode. The peaks in the diffraction pattern of each sample were analyzed using the software Diffrac (version 2.1). Then, the peaks were compared and matched with those of standard materials in the corresponding Powder Diffraction File (PDF-2, JCPDS International Center for Diffraction Data). A powder samples of the materials were analyzed using XRD and the peaks in diffraction pattern were compared to the Powder Diffraction File data. Results: Eight CSMs showed a similar diffraction pattern because their main component was calcium silicate. Eight CSMs showed similar diffraction peaks because calcium silicate was their main component. Two components were observed to have been added as radiopacifiers: bismuth oxide was detected in WMTA, OM, and EM while zirconium oxide was detected in RM, EN-Z, BD, EZ, and OM3. Unusual patterns were detected for the new material, OM3, which had strong peaks at low angles. Conclusion: It was caused by the presence of Brushite, which is believed to have resulted in crystal growth in a particular direction for a specific purpose.

The Synthesis of Maghemite and Hematite Nanospheres

  • Dar, Mushtaq Ahmad;Ansari, Shafeeque G.;Wahab, Rizwan;Kim, Young-Soon;Shin, Hyung-Shik
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2006.09a
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    • pp.472-473
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    • 2006
  • Maghemite and hematite nanospheres were synthesized by using the Sol-gel technique. The structural properties of these nanosphere powders were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), and pore size distribution. Hematite phase shows crystalline structures. The mean particle size that resulted from BET and XRD analyses were 4.9 nm and 2 nm. It can be seen from transmission electron microscopy that the size of the particles are very small which is in good agreement with the FESEM and the X-ray diffraction. The BET and pore size method were employed for specific surface area determination.

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An Study on the Structure of Maghemite(${\gamma}$-Fe$_2$O$_3$) I -Rietveld Analysis of Powder XRD Patterns- (마게마이트(${\gamma}$-Fe$_2$O$_3$)대한 연구 I -분말 X-선 회절무늬의 Rietveld 분석-)

  • 신형섭
    • Journal of the Korean Ceramic Society
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    • v.35 no.10
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    • pp.1113-1119
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    • 1998
  • Crystal structure of needle-shaped maghemite(${\gamma}$-{{{{ { {Fe }_{2 }O }_{3 } }}) has been studied by the Rieveld analysis of powder X-ray diffraction patterns. The tetragonal space group P41,.3212 and cubic space group P41,.32 have been have been used for the refinement of X-ray diffraction patterns. The crystal system of maghemite is closed to tetragonal more than cubic. The tetragonal lattice parameters are a=8.3460$\AA$ and c=25.034$\AA$ The standard X-ray diffraction pattern of the tetragonal maghemite analyzed with space group P41,.3212 is proposed.

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Determination of mixing ratios in a mixture via non-negative independent component analysis using XRD spectrum (XRD 스펙트럼의 비음독립성분분석을 통한 혼합물 구성비 결정)

  • You, Hanmin;Jun, Chi-Hyuck;Lee, Hyeseon;Hong, Jae-Hwa
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.502-507
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    • 2007
  • X-ray diffraction method has been widely used for qualitative and quantitative analysis of a mixture of materials since every crystalline material gives a unique X-ray diffraction pattern independently of others, with the intensity of each pattern proportional to that material's concentration in a mixture. For determination of mixing ratios, extracting source spectra correctly is important and crucial. Based on the source spectra extracted, a regression model with non-negativity constraint is applied for determining mixing ratios. In some mixtures, however, X-ray diffraction spectrum has sharp and narrow peaks, which may result in partial negative source spectrum from independent component analysis. We propose several procedures of extracting non-negative source spectra and determining mixing ratios. The proposed method is validated with experimental data on powder mixtures.