• Title/Summary/Keyword: XRD Diffraction

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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.

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.

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.

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.

Materials Characterization Using A Novel Simultaneous Near-Infrared/X-ray Diffraction Instrument

  • Yeboah, S.Agyare;Blanton, Thomas;Switalski, Steve;Schuler, Julie;Analytical, Craig Barnes
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1288-1288
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    • 2001
  • X-ray powder diffraction (XRD) is utilized for determination of polymorphism in crystalline organic materials. Though convenient to use in a laboratory setting, XRD is not easily adapted to in situ monitoring of synthetic chemical production applications. Near-Infrared spectroscopy (NIR) can be adapted to in situ manufacturing schemes by use of a source/detector probe. Conversely, NIR is unable to conclusively define the existence of polymorphism in crystalline materials. By combining the two techniques, a novel simultaneous NIR/XRD instrument has been developed. During material's analysis, results from XRD allow for defining the polymorphic phase present, and NIR data are collected as a fingerprint for each of the observed polymorphs. These NIR fingerprints will allow for the development of a library, which can be referenced during the use of a NIR probe in manufacturing settings.

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Characterization of few-layered reduced graphene oxide (rGO) for standardization (소수의 층을 갖는 환원 graphene oxide(rGO) 표준화를 위한 물성분석)

  • Ahn, Hae Jun;Huh, Seung Hun;Jee, Youngho;Lee, Byeong Woo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.6
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    • pp.239-245
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    • 2022
  • Reduced graphene oxide (rGO) has attracted many attention and applications due to its excellent electrochemical ability. Therefore, standardization of rGO through structural and thermal analysis facilitates quality improvement and management, enabling users to increase efficiency and reduce relevant costs. For rGO and graphene-related materials, it is very important to determine the number of layers and define the resulting difference in physical properties. In this study, 3~4 layers of rGO-1 and 9~10 layers of rGO-2 were obtained from graphene oxide (GO) through a hydrazine reduction process. For the prepared rGOs, X-ray diffraction (XRD) pattern obtained a diffraction peak at 2θ≈25° related to (002) reflection was used to calculate the layer numbers by determining interlayer distance and FWHM value. To reduce the angular uncertainty, XRD data analysis was performed with angle correction using standard reference materials for X-ray powder diffraction analysis. Precise interlayer distance and number of layers were determined using OriginLab and open-source XRD diffraction analysis programs using the angle-corrected diffraction data. TG-DSC thermal analysis was performed to further standardize the physical properties of rGO samples.

Ageing assessment of zirconia implant prostheses by three different quantitative assessment techniques

  • Kyaw, Phyu Phyu;Pongprueksa, Pong;Anuchitolarn, Warangkana;Sirinukunwatta, Krongkarn;Suputtamongkol, Kallaya
    • The Journal of Advanced Prosthodontics
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    • v.11 no.5
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    • pp.253-261
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    • 2019
  • PURPOSE. To evaluate the influence of cyclic loading on phase transformation of zirconia abutments and to compare the effectiveness of three different quantitative ageing assessment techniques. MATERIALS AND METHODS. Thirty two Y-TZP prostheses fabricated from two brands, InCoris ZI and Ceramill ZI, were cemented to titanium bases and equally divided into two subgroups (n=8): control group without any treatment and aged group with cyclic loading between 20 N and 98 N for 100,000 cycles at 4 Hz in distilled water at $37^{\circ}C$. The tetragonal-to-monoclinic phase transformation was assessed by (i) conventional x-ray diffraction (XRD), (ii) micro x-ray diffraction (${\mu}XRD$), and (iii) micro-Raman spectroscopy. The monoclinic-phase fractions (M%) were compared by two-way ANOVA. RESULTS. InCoris Zi presented significantly higher M% than Ceramill Zi in both control and aged groups (P<.001). Both materials exhibited significant phase transformation with monoclinicphase of 1 to 3% more in aged groups than controls for all three assessment techniques. The comparable M% was quantified by both ${\mu}XRD$ and XRD. The highest M% was assessed with micro-Raman. CONCLUSION. Cyclic loading produced significant phase transformation in tested Y-TZP prostheses. The micro-Raman spectroscopy could be used as an alternative to XRD and ${\mu}XRD$.

The Microstructure and physical properties of electroplated Cu films (열처리에 따른 Cu 전해도금막의 미세구조 및 물리적성질 변화)

  • 권덕렬;박현아;김충모;이종무
    • Journal of the Korean Vacuum Society
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    • v.13 no.2
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    • pp.72-78
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    • 2004
  • Cu seed layers deposited by magnetron sputtering onto tantalum nitride barrier films were treated with ECR plasma and then the copper films were electroplated and rapid thermal annealed in an argon or nitrogen atmosphere at various temperatures ranging from 200 to $500^{\circ}C$. Changes in the microstructure and physical properties of the copper films electroplated on the hydrogen ECR plasma cleaned copper seed layers were investigated using X-ray diffraction (XRD), electron back-scattered diffraction (EBSD), and atomic force microscopy (AFM) analyses. It was found that the copper film undergoes complete recrystallization during annealing at a temperature higher than $400^{\circ}C$. The resistivity of the Cu film tends to decrease and the degree of (111) preferred orientation tends to increase as the annealing temperature increases. Theoptimum annealing condition for obtaining the film with the lowest resistivity, the smoothest surface and the highest degree of the (111) preferred orientation is rapid thermal annealing in a nitrogen atmosphere at $400^{\circ}C$ for 120 s. The resistivity and the surface roughness of the electroplated copper film annealed under this condition are 1.98 $\mu$O-cm and 17.77 nm, respectively.

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.