• Macromolecular Research
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• v.13 no.6
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• pp.506-513
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• 2005

We review the recent SAXS activity on the 1.5-GeV electron storage ring at the National Synchrotron Radiation Research Center (NSRRC). Typical measurements featuring in grazing incident SAXS for soft materials are illustrated. Complex measurements using simultaneous SAXS/DSC and SAXSIWAXS for the correlations between the crystallization and mesoscale ordering in a polymer blend and a polypeptide-block-polypseudorotaxane diblock copolymer are presented. We also introduce a dedicated SAXS beamline which is planned at NSRRC.

• 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.

• Proceedings of the Korean Fiber Society Conference
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• 2001.10a
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• pp.417-419
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• 2001

폴리(트리메틸렌 테레프탈레이트)(PTT)와 폴리(트리메틸렌 나프탈레이트)(PTN)는 모두 방향족 폴리에스테르계 고분자들이지만 같은 계열의 다른 고분자에 비해 연구가 많이 진행되어 있지 않다 특히 PTT가 포함된 블렌드계의 경우 최근에 들어서야 방향족 다른 폴리에스테르계 고분자와의 블렌딩에 관한 몇가지 보고가 있을 뿐이다[1-3]. (중략)

• Fibers and Polymers
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• v.2 no.2
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• pp.98-107
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• 2001

The phase transition behavior isothermal micro-phase separation kinetics of polyester-based thermoplastic elastomer were studied using the synchrotron X-ray scattering(SAXS) method. The structural changes occurring during heating period were investigated by determining the changes of the one-dimensional correlation function, interfacial thickness and Porod constant. Based on the abrupt increases of the domain spacing and interfacial thickness, a major structural change occurring well below the melting transition temperature is suggested. Those changes are explained in terms of melting of the thermodynamically unstable hard domains or/and the interdiffusion of the hard and soft segments in the interfacial regions. SAXS profile changes during the micro-phase separation process were also clearly observed at various temperatures and the separation rate was found to be sensitively affected by the temperature. The peak position of maximum scattering intensity stayed constant during the entire course of the phase separation process. The scattering data during the isothermal phase separation process was interpreted with the Cahn-Hilliard diffusion equation. The experimental data obtained during the early stage of the phase separation seems to satisfy the Cahn-Hilliard spinodal mechanism. The transition temperature obtained from the extrapolation of the diffusion coefficient to zero value turned out to be about 147$\pm$$2^{\circ}$, which is close to the order-disorder transition temperature obtained from the Porod analysis. The transition temperature was also estimated from the inveriant growth rate. By extrapolating the inveriant growth rate to zero, a transition temperature of about 145$\pm$$\pm$$2^{\circ}$ was obtained.

• Macromolecular Research
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• v.12 no.1
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• pp.1-10
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• 2004

The structural changes occurring in the isothermal crystallization processes of polyethylene (PE), poly-oxymethylene (POM), and vinylidene fluoridetrifluoroethylene (VDFTrFE) copolymer have been reviewed on the basis of our recent experimental data collected by the time-resolved measurements of synchrotron-sourced wide-angle (WAXS) and small-angle X-ray scatterings (SAXS) and infrared spectra. The temperature jump from the melt to a crystallization temperature could be measured at a cooling rate of 600-1,000 $^{\circ}C$/min, during which we collected the WAXS, SAXS, and infrared spectral data successfully at time intervals of ca. 10 sec. In the case of PE, the infrared spectral data clarified the generation of chain segments of partially disordered trans conformations immediately after the jump. These segments then became transformed into more-regular all-trans-zigzag forms, followed by the formation of an orthorhombic crystal lattice. At this stage, the generation of a stacked lamella structure having an 800-${\AA}$-long period was detected in the SAXS data. This structure was found to transfer successively to a more densely packed lamella structure having a 400-${\AA}$-long period as a result of the secondary crystallization of the amorphous region in-between the original lamellae. As for POM, the formation process of a stacked lamella structure was essentially the same as that mentioned above for PE, as evidenced from the analysis of SAXS and WAXS data. The observation of morphology-sensitive infrared bands revealed the evolution of fully extended helical chains after the generation of lamella having folded chain structures. We speculate that these extended chains exist as taut tie chains passing continuously through the neighboring lamellae. In the isothermal crystallization of VDFTrFE copolymer from the melt, a paraelectric high-temperature phase was detected at first and then it transferred into the ferroelectric low-temperature phase at a later stage. By analyzing the reflection profile of the WAXS data, the structural ordering in the high-temperature phase and the ferroelectric phase transition to the low-temperature phase of the multi-domain structure were traced successfully.

• Proceedings of the Korean Fiber Society Conference
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• 1999.04a
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• pp.331-334
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• 1999

• Proceedings of the Korean Fiber Society Conference
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• 1999.10a
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• pp.369-372
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• 1999

• Macromolecular Research
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• v.13 no.6
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• pp.538-541
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• 2005

• Proceedings of the Korean Fiber Society Conference
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• 1996.10a
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• pp.376-378
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• 1996

• Proceedings of the Korean Fiber Society Conference
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• 2000.04a
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• pp.57-60
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• 2000