• Title/Summary/Keyword: XRD Analysis

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Estimation of Phase Ratio for TiO2 Powders by XRD and XAS (XRD와 XAS에 의한 TiO2 분말의 상분율 결정)

  • Rha, Sa-Kyun;Lee, Youn Seoung
    • Journal of the Korean Ceramic Society
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    • v.49 no.5
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    • pp.469-474
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    • 2012
  • The crystallinity and phase ratio of anatase to rutile in $TiO_2$ were estimated by x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS). Traditionally, the structural characterization of $TiO_2$ powders has been carried out by XRD techniques, which are comparatively easy in use and analysis. However, materials with amorphous phase, nano-sized or nano-structured crystallinities cannot be fully characterized by XRD because XRD analysis has a limit for abnormal contributions of the nano-crystal such as the surface contribution. From the comparison with the experimental and calculated Ti K-edge XAS spectra, we found the possibility of efficient estimation in the crystalinites and the phase ratio of anatase to rutile for nano-sized $TiO_2$ mixture.

XRD Analysis of Portland Limestone Cement Paste (포틀랜드 석회석 시멘트에 관한 XRD 분석)

  • Bang, Mi-Jin;Shin, Ki-Su;Park, Ki-Bong
    • Proceedings of the Korean Institute of Building Construction Conference
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    • 2018.05a
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    • pp.189-190
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    • 2018
  • This study produced Portland limestone cement at the rate of limestone substitution by grinding limestone and clinker together, and it conducted an XRD analysis to determine the sign language response structure as a basic study on Portland Limestone Cement. As a result of the XRD analysis, the higher the substitution rate of limestone, the more likely it is that the detection rate of ettringite is decreased. Additionally, we could see that the production volume of Mono-carbonate was increasing.

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Structural Study of the Oxidized High Modulus Carbon Fiber using Laser Raman Spectroscopy

  • Roh, Jae-Seung;Kim, Suk-Hwan
    • Carbon letters
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    • v.10 no.1
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    • pp.38-42
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    • 2009
  • This study aims to find a correlation between XRD and Raman result of the oxidized high modulus carbon fibers as a function of its oxidation degrees, and compare with the isotropic carbon fiber reported early. La of the high modulus carbon fiber prepared by oxidation in carbon dioxide gas have been observed using laser Raman spectroscopy. The basic structural parameters of the fibers were evaluated by XRD as well. The La of the original high modulus carbon fibers were measured to be 144 ${\AA}$ from Raman analysis and 135 ${\AA}$ from XRD analysis. La of the 92% oxidized fiber were 168 ${\AA}$ by using Raman and 182 ${\AA}$ by using XRD. There was some correlation between the La value obtained from Raman and XRD. However the La value changes of the high modulus carbon fiber through whole oxidation process showed opposite tendency compare with the isotropic carbon fiber because of the fiber structure basically.

Structural Study of the Activated Carbon Fiber using Laser Raman Spectroscopy

  • Roh, Jae-Seung
    • Carbon letters
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    • v.9 no.2
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    • pp.127-130
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    • 2008
  • This study aims to find a correlation between XRD and Raman result of the activated carbon fibers as a function of its activation degrees. La of the isotropic carbon fiber prepared by oxidation in carbon dioxide gas have been observed using laser Raman spectroscopy. The basic structural parameters of the fibers were evaluated by XRD as well, and compared with Raman result. The La of the carbon fibers were measured to be 25.5 ${\AA}$ from Raman analysis and 23.6 ${\AA}$ from XRD analysis. La of the ACFs were 23.6 ${\AA}$ and 20.4 ${\AA}$, respectively, representing less ordered through activation process. It seems that the $I_D/I_G$ of Raman spectra were related to crystallite size(La). Raman spectroscopy has demonstrated its unique ability to detect structural changes during the activation of the fibers. There was good correlation between the La value obtained from Raman and XRD.

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.

Quntitative Analysis of Calcium Carbonate Polymorphs by Peak Area of XRD (XRD 피크 면적을 이용한 탄산칼슘 결정 형태의 정량분석)

  • Bak, Young-Cheol
    • Korean Chemical Engineering Research
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    • v.60 no.4
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    • pp.564-573
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    • 2022
  • Calcium carbonate (CaCO3) exhibits three polymorphs: calcite with arhombohedral, vaterite with a spherical, and aragonite with a needle-like structure. Qualitative and quantitative analyses of the morphology of CaCO3 are very important to investigate the synthesis of single-crystal vaterite and aragonite. In this work, the polymorphs of calcium carbonate were quantitatively analyzed using XRD. Pure vaterite and pure aragonite were synthesized and the peak distribution of a single phase was analyzed. The vaterite fraction of a mixture of calcite and vaterite was calculated based on the intensity of a specific diffraction peak, and compared to the results based on the peak area. The mean value of fsV (the correction factor for the peak area of vaterite) was 0.654. The phase analysis of calcite-aragonite mixtures was performed, and the mean value of fsA (the correction factor for the peak area of aragonite) was obtained as 0.6713. Using these factors, Eq. (24)~Eq. (32) for the quantitative analysis based on the total peak area of XRD were derived to calculate the phase contents of ternary phase CaCO3. And three-component XRD section was defined considering overlapping sections.

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 ${\mu}XRD$.

Comparison of Analytical Methods for α-Quartz by FTIR and XRD (FTIR과 XRD를 이용한 α-Quartz 분석법 비교)

  • Kim, Boo-Wook;Lee, Jong-Seong;Choi, Byung-Soon
    • Journal of Environmental Health Sciences
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    • v.35 no.2
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    • pp.130-142
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    • 2009
  • This study compared FTIR with XRD method for the analysis of quartz by % recovery, coefficient of variation (CV) and influence of the interference. the results were as the following. 1. In FTIR method, the coefficient of determination ($r^2$) was 0.9998 in a calibration curve of $695\;cm^{-1}$, and the limit of detection was $4.9{\mu}g/sample$. 2. The highest recovery was $799\;cm^{-1}$ (98.2%). 3. The CVpooled of the FTIR method was approximately 10% in three wave numbers. 4. The analysis of qualitative and quantitative for quartz is difficult with mixed cristobalite and iron oxide. 5. In XRD method with rotating sample holder and LynxEye detector, the coefficient of determination was 0.9996 in a calibration curve, and the limit of detection was $5.9{\mu}g/sample$. 6. The recovery and CV pooled were 104.3%, and 11 %, respectively. 7. In muffle furnace ashing, the quartz weight decreased to 34% when the maximum weight of the iron oxide was more than eight times. In conclusion, the accuracy (% recovery) and precision (CV) of FTIR and XRD method for analyzing $\alpha$-quartz were similar. FTIR method was a disadvantage for sample matrix because it indicates possibility of interference. However, XRD method distinguished specific crystalline forms of silica, and the majority of silicate minerals. In addition, XRD method recommend filter dissolution to pretreatment method.

Properites of Inorganic Hybrid Silica Materials according to the XRD patterns (XRD 패턴에 따른 유무기복합 화합물의 특성)

  • 오데레사;고유신;김경식
    • Proceedings of the IEEK Conference
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    • 2003.07b
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    • pp.995-998
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    • 2003
  • This paper reports the correlation between dielectric constant and degree of amorphism of the hybrid type Si-O-C thin films. Si-O-C thin films were deposited by high density plasma chemical vapor deposition using bistrimethyl- silylmethane(BTMSM, $H_{9}$C$_3$-Si-C $H_2$-Si-C$_3$ $H_{9}$) and oxygen precursors with various flow rate ratio. As-deposited film and annealed films at 40$0^{\circ}C$ were analyzed by XRD. The Si-O-C 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.

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