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

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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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Fire Performance Testing Method for Fire Retardant EPS Sandwich Panel Using X-ray Analysis (X-선 분석법을 이용한 난연 EPS 샌드위치 패널의 화재성능평가 방법에 관한 연구)

  • Shim, Ji-Hun;Cho, Nam-Wook
    • Fire Science and Engineering
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    • v.29 no.6
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    • pp.76-83
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    • 2015
  • EPS sandwich panel contains flame retardants that slow down ignition during fires,reduce the amount of heat generated, and block the spread of combustion. However, if a sandwich panel does not satisfy standards for fire-retardant performance, it may increase damage to property and human life. It is difficult to test the fire-retardant performance of a finishing material with the naked eye, so it is necessary to develop convenient and fast evaluation methods that are convenient and fast. In this study, a fire safety evaluation method for EPS sandwich panel was analyzed using X-ray to detect specific components related to the fire-retardant performance X-ray fluorescence analysis (XRF) indicated that suitable panel products contained more aluminum in comparison to unsuitable products. Gibbsite was identified as the main crystalline material of flame retardant EPS through X-ray diffraction analysis (XRD) and was included in both suitable products and unsuitable products, but there was a difference in crystalline structure. This study was verifies the possibility of evaluating fire-retardant performance using ultimate analysis and crystal analysis through these X-ray methods.

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.

Mineral Properties of Yangsan.Mulkum Clay (양산물금 점토의 광물학적 특성)

  • 정하익;이용수;진규남;진현식
    • Proceedings of the Korean Geotechical Society Conference
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    • 1999.10a
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    • pp.75-80
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    • 1999
  • In this study, clay sampled from Yangsan$.$Mulkum site were used to analyze mineral properties. Mineral and chemical properties of clay were investigated through X-ray fluorescence spectrometer(XRF), X-Ray Diffraction(XRD), and Scanning Electron Microscope(SEM) analysis. The result of this test represents that Yangsan$.$Mulkum clay are composed of quartz, albite, anorthite, orthocalse and illite.

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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 ${\mu}XRD$.

Interfacial Natures and Controlling Morphology of Co Oxide Nanocrystal Structures by Adding Spectator Ni Ions

  • Gwag, Jin-Seog;Sohn, Young-Ku
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.505-510
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    • 2012
  • Cobalt oxide nanostructure materials have been prepared by adding several concentrations of spectator Ni ions in solution, and analyzed by electron microscopy, X-day diffraction, calorimetry/thermogravimetric analysis, UV-vis absorption, Raman, and X-ray photoelectron spectroscopy. The electron microscopy results show that the morphology of the nanostructures is dramatically altered by changing the concentration of spectator ions. The bulk XRD patterns of $350^{\circ}C$-annealed samples indicate that the structure of the cobalt oxide is all of cubic Fd-3m $Co_3O_4$, and show that the major XRD peaks shift slightly with the concentration of Ni ions. In Raman spectroscopy, we can confirm the XRD data through a more obvious change in peak position, broadness, and intensity. For the un-sputtered samples in the XPS measurement process, the XPS peaks of Co 2p and O 1s for the samples prepared without Ni ions exhibit higher binding energies than those for the sample prepared with Ni ions. Upon $Ar^+$ ion sputtering, we found $Co_3O_4$ reduces to CoO, on the basis of XPS data. Our study could be further applied to controlling morphology and surface oxidation state.

7Li-NMR and Thermal Analysis for Lithium Inserted into Artificial Carbon Material

  • O, Won Chun
    • Bulletin of the Korean Chemical Society
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    • v.22 no.4
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    • pp.367-371
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    • 2001
  • Lithium inserted into artificial carbon has been synthesized as a function of the Li concentration. The characteristics of these prepared compounds were determined from the studies using X-ray diffraction(XRD), solid nuclear magnetic resonance (NM R) spectrophotometric and differential scanning calorimeter(DSC) analysis. X-ray diffraction showed that lower stage intercalation compounds were formed with increasing Li concentration. In the case of the AG3, most compounds formed were of the stage 1 structure. Pure stage 1 structural defects of artificial graphite were not observed. 7Li-NMR data showed that bands are shifted toward higher frequencies with increasing lithium concentration; this is because non-occupied electron shells of Li increased in charge carrier density. Line widths of the Li inserted carbon compounds decreased slowly because of nonhomogeneous local magnetic order and the random electron spin direction for located Li between graphene layers. The enthalpy and entropy changes of the compounds can be obtained from the differential scanning calorimetric analysis results. From these results, it was found that exothermic and endothermic reactions of lithium inserted into artificial carbon are related to the thermal stability of lithium between artificial carbon graphene layers.

Asbestos Determination of Some Domestic Building-Materials Using X-ray diffraction (국내 건축자재에 함유된 석면의 함량에 대한 X-선회절분석 연구)

  • Hwang, Jin-Yeon;Lee, Hyo-Min;Oh, Ji-Ho;Park, Gi-Nam
    • Journal of the Mineralogical Society of Korea
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    • v.24 no.2
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    • pp.119-131
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    • 2011
  • The asbestos contents in some representative building materials were analyzed using JIS (Japanese Industrial Standard) X-ray diffraction (XRD) method. The changes in mineral composition during analysis process and problems in JIS method were also examined. XRD analysis of some representative domestic building materials used for roof, wall, ceiling, and floor indicates that slate have the highest asbestos content having 6.87~6.93% of chrysotile. Other building materials analyzed in this study also have 1.35~3.98% of chrysotile contents. The XRD analysis results of asbestos contents in some domestic building materials are presented in this study. This method is very effective for the asbestos content evaluation of building materials according to newly modified asbestos content regulation (Law of Industrial Safety and Health, 2007-26) that limits asbestos content less than 0.1% by Ministry of Employment and Labor. Small amount of tremolite as well as chrysotile were also observed in some samples. With consideration of crystal shape, contents and geological occurrence, it is considered that tremolite is an associated mineral of chrysotile and is not intentionally added. Complemental analyses with optical microscope and SEM/EDS are also necessary because XRD method cannot distinguish asbestiform from non-asbestiform. The XRD method applied in this study is very effective in the asbestos content analysis of building materials, specially building materials showing high asbestos concentration in residues due to the high loss rate with ashing and acid dissolution procedure.

Analysis of CaCO3 structure of marine bivalves using X-ray diffraction (해산 이매패류 패각의 CaCO3 결정 구조에 대한 X-ray 회절 분석)

  • Nam, Ki-Woong;Lee, Seng-Woo;Song, Jae-Hee;Jeung, Hee-Do;Park, Kyung-Il
    • The Korean Journal of Malacology
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    • v.31 no.4
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    • pp.279-283
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    • 2015
  • This study investigated spectroscopic characteristics of shell crystals of eight marine bivalve species using X-ray diffraction (XRD) analysis; moreover, the Family level relatedness of shellfish was investigated. In XRD analysis, the shells of Ruditapes philippinarum, Meretrix lusoria, Anadara granosa, and Fulvia mutica were found to have orthorhombic aragonite $CaCO_3$ crystals, while shells of Patinopecten yessoensis and Crassostrea gigas had trigonal-rhombohedral calcite crystals. The shells of Mytilus coruscus and Atrina pectinata were determined to have a mixture of aragonite and calcite crystals. XRD information revealed the Family level-specific characteristics of shellfish; the results agreed with the current taxonomic system. In conclusion, spectroscopic characteristics of shell crystals indicated Family-level characteristics of shellfish and suggested a more intense species-level investigation; this technology may be useful in identifying shellfish species using small quantities of shells.

Activation energy for the loss of substitutional carbon in $Si_{0.984}C_{0.016}$ grown by solid phase epitaxy

  • Kim, Yong-Jeong;Kim, Tae-Joon;Park, Byungwoo;Song, Jong-Han
    • Journal of Korean Vacuum Science & Technology
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    • v.4 no.2
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    • pp.50-54
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    • 2000
  • We studied the synthesis of S $i_{1-x}$ Cx (x=0.016) epitaxial layer using ion implantation and solid phase epitaxy (SPE). The activation energy Ea was obtained for the loss of substitutional carbon using fourier transform-infrared spectroscopy (FTIR) and high-resolution x-ray diffraction (HR-XRD). In FTIR analysis, the integrated peak intensity was used to quantify the loss of carbon atoms from substitutional to interstitial sites during annealing. The substitutional carbon contents in S $i_{0.984}$ $C_{0.016}$ were also measured using HR-XRD. By dynamic simulations of x-ray rocking curves, the fraction of substitutional carbon was obtained. The effects of annealing temperature and time were also studied by comparing vacuum furnace annealing with rapid thermal annealing (RTA))))))

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