• Title/Summary/Keyword: small-angle X-ray scattering

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Current Status of the Synchrotron Small-Angle X-ray Scattering Station BL4C1 at the Pohang Accelerator Laboratory

  • Jorg Bolze;Kim, Jehan;Huang, Jung-Yun;Seungyu Rah;Youn, Hwa-Shik;Lee, Byeongdu;Shin, Tae-Joo;Moonhor Ree
    • Macromolecular Research
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    • v.10 no.1
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    • pp.2-12
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    • 2002
  • The small-angle X-ray scattering (SAXS) beamline BL4C1 at the 2.5 GeV storage ring of the Pohang Accelerator Laboratory (PAL) has been in its first you of operation since August 2000. During this first stage it could meet the basic requirements of the rapidly growing domestic SAXS user community, which has been carrying out measurements mainly on various polymer systems. The X-ray source is a bending magnet which produces white radiation with a critical energy of 5.5 keV. A synthetic double multilayer monochromator selects quasi-monochromatic radiation with a bandwidth of ca. 1.5%. This relatively low degree of monochromatization is sufficient for most SAXS measurements and allows a considerably higher flux at the sample as compared to monochromators using single crystals. Higher harmonics from the monochromator are rejected by reflection from a flat mirror, and a slit system is installed for collimation. A charge-coupled device (CCD) system, two one-dimensional photodiode arrays (PDA) and imaging plates (IP) are available its detectors. The overall performance of the beamline optics and of the detector systems has been checked using various standard samples. While the CCD and PDA detectors are well-suited for diffraction measurements, they give unsatisfactory data from weakly scattering samples, due to their high intrinsic noise. By using the IP system smooth scattering curves could be obtained in a wide dynamic range. In the second stage, stating from August 2001, the beamline will be upgraded with additional slits, focusing optics and gas-filled proportional detectors.

Crystallization Behavior of Polymers as Viewed from the Molecular Level

  • Tashiro, Kohji;Sasaki, Sono;Ueno, Yoko;Yoshioka, Akiko;Kobayashi, Masamichi
    • Macromolecular Research
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    • v.8 no.3
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    • pp.103-115
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    • 2000
  • The structural changes viewed from the molecular level have been investigated for the isothermal crystallization phenomena of polyethylene (PE) and the solvent-induced crystallization phenomenon of syndiotactic polystyrene (sPS) glassy sample. The data, which were collected by the time-resolved measurements of Fourier-transform infrared spectra, Raman spectra, synchrotron-sourced small-angle X-ray scattering, wide-angle X-ray scattering, and so on, were combined together to extract the detailed structural information in these phase transition phenomena. In the case of PE, the isothermal crystallization from the melt to the orthorhombic form was found to occur via the conformationally-disordered trans chain form, followed by the formation of the lamellar stacking structure of regular orthorhombic-type crystals. In the case of sPS, the amorphous chains in the glassy sample were found to enhance the mobility through the interaction with the injected solvent molecules, which act as a trigger to cause the conformational ordering from the random coil to the regular T$_2$G$_2$-type helical form. The thus created short helical segments were found to grow into longer helices, which gathered together to form the crystallites, as revealed by the organized coupling of the infrared, Raman and X-ray scattering data.

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Small Angle X-Ray Scattering Study on the Oxopolymer Variations of BaTi-ethoxide Sol by Catalysts (촉매제에 의한 BaTi-에톡사이드 솔의 옥소폴리머 변화에 대한 저각 X선 산란연구)

  • 고태경;배호기
    • Korean Journal of Crystallography
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    • v.4 no.1
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    • pp.36-41
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    • 1993
  • Small angle X-ray scattering was used to study on the oxopolymers of sols derived from BaTiethoxide. The growths of the oxopolymers in tools obtained with NH40H as catalyst and catalystfree sol are similar. Their radii of gyration are 1.66-2.08nm. They exhibit a mass fractal behavior with a dimension of 1.6, which is almost inde pendent with amount of NH40H addition. Sols catalyzed with CHSCOOH have greater radii of gyration of 3.24-4.OOnm. Their scattering curves are similar in the intermediate Q region, showing a mass fractal dimension of 1.8. The oxopolymers of the tools from the base and the neutral hydrolysis conditions may have a short chain structure.

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Structure Analyses of Rubber/Filler System under Shear Flow by Using Time Resolved USAXS Method

  • Nishitsuji, Shotaro;Takenaka, Mikihito;Amino, Naoya;Ishikawa, Yasuhiro
    • Elastomers and Composites
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    • v.54 no.2
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    • pp.156-160
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    • 2019
  • The changes in the dispersion of carbon black in liquid polyisoprene under shear flow with time have been investigated by time-resolved ultra small-angle X-ray scattering (USAXS) method. The analyses of USAXS profile immediately after the start of shear flow clarified that the aggregates of carbon black with a mean radius of gyration of 14 nm and surface fractal dimension of 2.5 form the fractal network structure with mass-fractal dimension of 2.9. After the application of the shear flow, the scattering intensity increases with time at the observed whole entire q region, and then the a shoulder appears at $q=0.005nm^{-1}$, indicating that the agglomerate is broken and becomes smaller by shear flow. The analysis by the Unified Guinier/Power-law approach yielded several characteristic parameters, such as the sizes of aggregate and agglomerate, mass-fractal dimension of agglomerate, and surface fractal dimension of the primary particle. While the mean radius of gyration of the agglomerate decreases with time, the mean radius of gyration of the aggregate, mass fractal dimension, and surface fractal dimension don't change with time, indicating that the aggregates peel off the surface of the agglomerate.

Melting Behavior of Uni-Axially Deformed Polyethylenes Containing Comonomers as Studied by in-situ Small and Wide Angle X-ray Scattering (실시간 소각 밑 광각 X-선 산란을 이용한 일축 변형된 공단량체 함유 폴리에틸렌의 용융 거동)

  • Cho, Tai-Yon;Jeon, Hye-Jin;Ryu, Seok-Gn;Song, Hyun-Hoon
    • Polymer(Korea)
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    • v.33 no.2
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    • pp.183-188
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    • 2009
  • Structural rearrangements of uni-axially deformed polyethylenes containing 1-octene comonomer and HDPE upon heating were investigated by time-resolved small and wide angle X-ray scattering techniques. During heating, structural changes including crystal transformation and lamellar rearrangement noted were very different depending on the comonomer contents. At low comonomer content below 2 wt%, inverse martensitic transformation of crystal lattice from monoclinic to orthorhombic cell and the rearrangement of broken lamellar units into more ordered and perfect lamellar stacks were noted with the temperature increase. At high contents above 9.5 wt%, however, polyethylene copolymers showed neither the crystal transformation nor lamellar rearrangement that can be attributed to low crystallinity and high content of branch units.

Competition between Phase Separation and Crystallization in a PCL/PEG Polymer Blend Captured by Synchronized SAXS, WAXS, and DSC

  • Chuang Wei-Tsung;Jeng U-Ser;Sheu Hwo-Shuenn;Hong Po-Da
    • Macromolecular Research
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    • v.14 no.1
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    • pp.45-51
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    • 2006
  • We conducted simultaneous, small-angle, X-ray scattering/differential scanning calorimetry (SAXS/DSC) and simultaneous, wide-angle, X-ray scattering (WAXS)/DSC measurements for a polymer blend of poly($\varepsilon$-caprolactone)/poly(ethylene glycol)(PCL/PEG). The time-dependent SAXS/DSC and WAXS/DSC results, measured while the system was quenched below the melting temperature of PCL from a melting state, revealed the competitive behavior between liquid-liquid phase separation and crystallization in the polymer blend. The time-dependent structural evolution extracted from the SAXS/WAXS/DSC results can be characterized by the following four stages in the PCL crystallization process: the induction (I), nucleation (II), growth (III), and late (IV) stages. The influence of the liquid-liquid phase separation on the crystallization of PCL was also observed by phase-contrast microscope and polarized microscope with 1/4$\lambda$ compensator.

Sol-Gel Transition in Di-(2-ethylhexyl) phthalate-Plasticized Poly(vinyl chloride)

  • Lee, Chang-Hyung;Nah, Jae-Woon;Cho, Kil-Won;Kim, Seong-Hun;Hahn, Ai-Ran
    • Bulletin of the Korean Chemical Society
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    • v.24 no.10
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    • pp.1485-1489
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    • 2003
  • The gelation for di-(2-ethylhexyl) phthalate (DEHP)-plasticized poly(vinyl chloride) was studied by measuring time-resolved small-angle X-ray scattering (SAXS) and a flow of the solutions in test tube. It was found that for the gelation there were three regimes. At Regime I, the solution rapidly changed to a gel, and the SAXS intensity showed a peak and the peak intensity increased, keeping the peak angle constant. Applying the SAXS intensity to the kinetic analysis of the liquid-liquid phase separation, it was revealed that the spinodal decomposition proceeded to develop a periodic length of 29.9 nanometer in size, a hydrogen-bonding-type association in polymer rich phase followed, and then it induced fast gelation rate. At Regime II, the gelation slowly occurred and the SAXS intensity was not observed, suggesting that a homogeneous gel network was formed by a hydrogen-bonding. At regime III, the solution was a homogeneous sol.