• 제목/요약/키워드: x-ray diffraction(XRD)

검색결과 2,640건 처리시간 0.027초

The Structure Determination of La2/3-xLi3x1/3-2xTiO3 by the Powder Neutron and X-ray Diffraction

  • Kang, Eun-Tae;Kwon, Young-Jean
    • 한국세라믹학회지
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    • 제40권6호
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    • pp.513-518
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    • 2003
  • La/sub 2/3-x/Li/sub 3x/□/sub 1/3-2x/TiO₃ compounds with x=0.13 and 0.12 were prepared by slow cooling (x=0.13) and rapid quenching (x=0.12) into the liquid nitrogen after sintering at 1350℃ for 6 h. Their crystal structure has been determined by Rietveld refinement of both the powder neutron and X-ray diffraction data. From neutron diffraction data, we found that the main phase was not tetragonal (P4/mmm), but trigonal (R3cH). The refinement of neutron diffraction for the slow cooled samples were in a good agreement with a new model; a mixture of trigonal (R3cH, 45.7 wt%), tetragonal (p4/mmm, 37.0 wt%), and Li/sub 0.57/Ti/sub 0.86/O₂(pbnm, 17.2 wt%), but the quenched sample was found not to contain tetragonal (p4/mmm). X-ray diffraction data couldn't be well fitted because of the Poor scattering factor of lithium ions and the similar reflection patterns among trigonal (R3cH), tetragonal (p4/mmm), and cubic (Pm3m). We also knew that one transport bottlenecks is destroyed by one La vacancy in the case of trigonal (R3cH).

FT-IR and X-Ray Diffraction Characterization of Melanoidins Formed from Glucose and Fructose with Amino Acid Enantiomers in the Maillard Reaction

  • Kim, Ji-Sang;Lee, Young-Soon
    • Food Science and Biotechnology
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    • 제18권2호
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    • pp.546-551
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    • 2009
  • The objective of this study was to investigate Fourier transform infrared (FT-IR) spectrometry and the X-ray diffraction (XRD) characterization of melanoidins formed from glucose and fructose with amino acid enantiomers in the Maillard reaction. Before dialysis, FT-IR spectroscopy of all the samples showed that the characteristic absorption intensities appeared as a broad and intense band of the stretching vibration of the -OH group at 3,400/cm for a high pH. The absorption bands of the melanoidins sharply decreased in intensity after dialysis as compared to those before dialysis. In particular, the absorption bands at 992 and 575/cm disappeared. The XRD confirmed that the crystal structure of the melanoidins disappeared after dialysis and a new crystal structure was formed at 9 and $28^{\circ}$ ($2{\theta}$. In particular, broad diffraction peaks were formed in the $10-21^{\circ}$ ($2{\theta}$) range for a high pH, while other sharp diffraction peaks disappeared.

Synchrotron X-Ray Diffraction Studies on Crystalline Domains in Urea-Formaldehyde Resins at Low Molar Ratio

  • WIBOWO, Eko Setio;PARK, Byung-Dae;CAUSIN, Valerio;HAHN, Dongyup
    • Journal of the Korean Wood Science and Technology
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    • 제50권5호
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    • pp.353-364
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    • 2022
  • The crystalline domain of thermosetting urea-formaldehyde (UF) resins at low formaldehyde-to-urea (F/U) molar ratios (≤ 1.0) is known to be responsible for their poor performance as wood adhesives. Crystallization has been observed in 1.0 F/U UF resins during the addition reaction stage and at the end of the synthesis process (neat UF resins). The crystallinity and X-ray diffraction (XRD) spectra of the uncured neat UF resins, on the other hand, differed significantly from those of the cured neat UF resins, raising the possibility that their crystal structures were also different. This study demonstrates for the first time that the crystalline domains in 1.0 F/U UF resins generated from uncured and cured samples are identical. Despite having a lower crystallinity value, the synchrotron XRD patterns of purified neat UF resins were equivalent to the XRD patterns of cured neat UF resins. Transmission electron microscope images of the cured UF resins showed that the crystals were lamellar structures. This finding suggests that the crystal at low molar ratio UF resins are isotropic polycrystals with random orientation.

RAMBE를 사용하여 Si 기판 위에 성장된 AIN 박막의 결정성 분석 (Microstructural ananalysis of AlN thin films on Si substrate grown by plasma assisted molecular beam epitaxy)

  • 홍성의;한기평;백문철;조경익;윤순길
    • 한국진공학회지
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    • 제10권1호
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    • pp.22-26
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    • 2001
  • Plasma assisted molecular beam epitaxy(PAMBE)를 사용하여 Si 기판위에 성장시킨 AlN 박막에 대하여 성장온도 및 기판의 방향성에 따른 박막의 결정성 변화를 분석하였다. Reflection high energy electron diffraction(RHEED) 패턴을 이용하여 성장 중의 결정성을 관찰하였고, 성장 후에는 X-ray diffraction(XRD), double crystal X-ray diffraction(DCXD), transmission electron microscopy/diffraction(TEM/TED)분석을 하였다. $850^{\circ}C$이상의 온도에서 Si(100)위에 성장된 AlN박막은 육방정계의 c축 방향으로 우선 배향되어 있음을 확인하였으며 Si(111)위에 성장된 AlN박막의 경우 AlN(0001)/Si(111), AlN(1100)/Si(110), AlN(1120)/Si(112)의 결정방위를 가지고 성장하였음을 확인하였다. 또한 Si(111) 기판 위에서는 전위와 적층결함 등 많은 결정결함에 의해 DCD패턴의 반치폭이 2$\theta$=$36.2^{\circ}$에서 약 3000arcsec에 이르는 등 결정성은 좋지 않았으나 AlN박막이 단결정으로 성장된 것으로 나타났다.

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Insight Into the Crystallinity of Chinese Ancient Silk by Synchrotron Radiation-Based and Conventional X-ray Diffraction Methods

  • Gong, Decai;Zhang, Xiaoning;Gong, Yuxuan
    • 보존과학회지
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    • 제36권1호
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    • pp.1-14
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    • 2020
  • This study investigates the crystallinity distribution of ancient silk. Owing to the inherent multi-hierarchical structure of silk protein and the complicated structural changes that occur due to various burial environments, it is challenging but worthwhile to study ancient silk ageing behavior, which is based on the fact that ageing begins with a single fiber and then spreads to a whole fabric. Crystallinity was one of the most effective indicators found to reveal the ageing status of silk. Therefore, a synchrotron radiation-based X-ray diffraction(SR-XRD) method was employed to study the crystallinity distribution of single fibers of ancient silk unearthed from seven archaeological sites in China from historical periods including the warring states, Han dynasty, Song dynasty, and Ming dynasty. In comparison, the conventional X-ray diffraction method, which uses large amounts of samples, was also performed to determine the integral crystallinity of ancient silk. Thermal stability experiments by thermogravimetry(TG) as well as morphology observations by scanning electron microscopy(SEM) and optical microscopy(OM) all confirmed the deterioration of ancient silk. Moreover, the ageing mechanism of ancient silk was proposed with the assistance of an artificial ageing study. The results confirmed the effectiveness of SR-XRD as an ageing indicator, revealing the crystallinity distribution. This research could provide motivation to determine the deterioration status of ancient silk, and would also aid in explaining the fragility of ancient silk due to ageing.

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

  • Yeboah, S.Agyare;Blanton, Thomas;Switalski, Steve;Schuler, Julie;Analytical, Craig Barnes
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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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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Ru를 도입한 TiO2의 합성과 산소를 이용한 알코올 산화반응 연구 (Synthesis of Ru Incorporated TiO2 and Application to Oxidation of Benzyl Alcohol with Molecular Oxygen)

  • 김영용;최명룡;권기영
    • 공업화학
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    • 제25권6호
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    • pp.645-647
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    • 2014
  • 본 연구에서는 수열합성법을 이용하여, 한단계의 과정으로 $TiO_2$와 Ru (Ruthenium)가 도입된 $TiO_2$ ($Ru_x/TiO_2$)를 합성하였다. 합성된 샘플의 결정성과 조성 및 형태를 X-ray diffraction (XRD)과 energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM)를 통하여 확인하였으며, Benzyl alcohol의 Benzaldehyde로의 산화반응에 촉매로서 적용하였다. 높은 선택성을 가지는 산화반응이 진행되었으며, $TiO_2$에 도입된 Ru의 양이 증가할수록 촉매로서의 더 좋은 촉매활성을 보였다.

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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    • 제33권2호
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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.

X-선 회절 분석을 통한 고온 피해 시멘트 경화체의 성분 변화 분석 (Analysis of the Changes of composition of Hardened Cement at High Temperature by X-Ray Diffraction)

  • 지우람;박지웅;신기돈;이건철;허영선
    • 한국건축시공학회:학술대회논문집
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    • 한국건축시공학회 2017년도 추계 학술논문 발표대회
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    • pp.113-114
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    • 2017
  • In this study, the change of composition of cement hardened at high temperature through XRD was observed. The specimen was made of cement paste and the heating rate condition was applied at rapid thermal annealing (10.0℃ / min). The decrease of calcium hydroxide was not confirmed, but the calcium carbonate tended to be impossible or decreased after 800℃. Calcium silicate and larnite were observed to increase with increasing temperature. It is considered that silicic acid, which is a stable structure due to the decomposition of calcium silicate, is changed into a phase such as lime.

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Polypropylene Reactive Nanocomposites with Functional Nanoclays

  • Phandee, Atinuch;Magaraphan, Rathanawan;Nithitanakul, Manit;Manuspiya, Hathaikarn
    • 한국고분자학회:학술대회논문집
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    • 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
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    • pp.280-280
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    • 2006
  • Na-bentonite (local clay mineral) and Na-montmorillonite were treated with quaternary alkylammonium cations. The effect of the molecular structure and functional groups of the surfactants on the organoclays was investigated by X-ray diffraction (XRD). For the preparation of nanocomposites, organoclays were melt-blended with polypropylene in a twin screw extruder and $Surlyn^{(R)$. ionomer was used as a reactive compatibilizer. The clay dispersions in the composites were investigated by X-ray diffraction (XRD). XRD spectra showed no peak at low angle indicated that the silicate clay layer has a nearly exfoliated dispersion in the polymer matrix. Thermal and mechanical properties of nanocomposites were higher than those of PP.

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