• 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.

• 한국신재생에너지학회:학술대회논문집
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• 2009.06a
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• pp.282-285
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• 2009

This study presents preparation and characterization of composite membranes based on ionic liquids. The ionic liquids act as water in sulfonated membranes. On the behalf of ionic conduction through ionic liquid inside the membranes, non-aqueous membranes showed Arrenhius dependence on temperature with no external humidification. It was implied that hopping mechanism of proton was dominant in the ionic liquid based membranes. In addition, small angle X-ray (SAXS) studies provided the information on morphology of ionic clusters formed by the interaction between sulfonic acid groups of the polymers and ionic liquids. The SAXS spectra showed matrix peaks, ionomer peaks and Prodo's law for Nafion based composite membranes and only matrix peaks for hydrocarbon based ones. However, ionic conductivity and atomic force microscopy (AFM) images showed the clear formation of ionic clusters of the hydrocarbon based composite membranes. It implies for ionic liquid based high temperature membranes that it is important to use sulfonated polymers as solid matrix of ionic liquid which can form clear ionic clusters in SAXS spectra.

• Macromolecular Research
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• v.15 no.7
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• pp.662-670
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• 2007

The crystallization behavior and fine structure of poly(ethylene terephthalate) (PET)/A-zeolite nanocomposites were assessed via differential scanning calorimetry (DSC) and time-resolved small-angle X-ray scattering (TR-SAXS). The Avrami exponent increased from 3.5 to approximately 4.5 with increasing A-zeolite contents, thereby indicating a change in crystal growth formation. The rate constant, k, evidenced an increasing trend with increases in A-zeolite contents. The SAXS data revealed morphological changes occurring during isothermal crystallization. As the zeolite content increased, the long period and amorphous region size also increased. It has been suggested that, since PET molecules passed through the zeolite pores, some of them are rejected into the amorphous region, thereby resulting in increased amorphous region size and increased long period, respectively. In addition, as PET chains piercing into A-zeolite pores cannot precipitate perfect crystal folding, imperfect crystals begin to melt at an earlier temperature, as was revealed by the SAXS profiles obtained during heating. However, the spherulite size was reduced with increasing nanofiller content, because impingement between adjacent spherulites in the nanocomposite occurs earlier than that of homo PET, due to the increase in nucleating sites.

• Bulletin of the Korean Chemical Society
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• v.23 no.4
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• pp.580-586
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• 2002

We investigated the effect of ionic component on crystalline morphology development during isothermal annealing in a sodium neutralized sulfonated poly(ethylene terephthalate) ionomer (Ion-PET) by time-resolved small-angle x-ray scattering (TR-SAX S) using synchrotron radiation. At early stage in Ion-PET, SAXS intensity at a low annealing temperature (Ta = 120 $^{\circ}C)$ decreased monotonously with scattering angle for a while. Then SAXS profile showed a peak and the peak position progressively moved to wider angles with isothermal annealing time. Finally, the peak intensity decreased, shifting the peak angle to wider angle. It is revealed that ionic aggregates (multiplets structure) of several nm, calculated by Debye-Bueche plot, are formed at early stage. They seem to accelerate the crystallization rate and make fine crystallites without spherulite formation (supported by optical microscopy observation). From decrease of peak intensity in SAXS,it is suggested that new lamellae are inserted between the preformed lamellae so that the concentration of ionic multiplets in amorphous region decreases to lower the electron density difference between lamellar crystal and amorphous region. In addition, analysis on the annealing at a high temperature (Ta = 210 $^{\circ}C)$ by optical microscopy, light scattering and transmission electron microscopy shows a formation of spherulite, no ionic aggregates, the retarded crystallization rate and a high level of lamellar orientation.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.47 no.1
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• pp.85-92
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• 2021

The stratum corneum is formed from keratinocytes and intercellular lipids, with ceramide as the main component of intercellular lipids. Ceramides are one of the important components of the intercellular lipids to form a lamellar structure, but they are insoluble and therefore are not suitable for direct application to the skin. Thus, it was intended to apply ceramide to the formulation of pluronic lecithin organogel (PLO gel), which received constant attention among drug delivery systems. A suitable oil for formulation was selected and a PLO gel containing ceramide was manufactured. Liquid crystal formation and variation were observed using polarized microscopes, and viscoelastic analysis was performed to find out the viscoelastic behavior of the PLO gel. Small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) analysis were performed to confirm the structures in the formulation. Results showed that the size and stability of the liquid crystal differed depending on the content ratio of ceramide and lecithin in the PLO gel containing ceramide. Furthermore, viscoelastic analysis showed the stability of the formulation, and SAXS/WAXS analysis confirmed that the PLO gel without ceramide had hexagonal structure of the quadrilateral system array, and the PLO gel with ceramide had the lamellar structure of the quadrilateral system array.

• 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

• Proceedings of the Korean Fiber Society Conference
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• 1995.04a
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• pp.28-29
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• 1995

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