• 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.

• 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.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.44 no.4
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• pp.43-50
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• 2012

The crystallinity index is an important characteristic of cellulose. The crystallinity value is different depending on the adopted instrument. In this study, we determined a crystallinity index of cotton and wood celluloses using wide-angle X-ray scattering (WAXS), powder X-ray diffractometer (PXRD), and cross polarization/magic angle spinning solid-state $^{13}C$ nuclear magnetic resonance spectroscopy (CP/MAS solid-state $^{13}C$ NMR). The specimen was prepared in forms of powder, sheet and pallet. With the comparison of the obtained crystallinity indices of the cellulose, the effects of the analysis instrument, the sample preparation and analysis method were investigated. Among three instruments, the crystallinity indices by PXRD and NMR had a good relationship and reproducibility, and WAXS gave the crystallinity index with poor reproducibility. In the case of analysis methods of crystallinity indices, the Segal method showed higher value than that of the Ruland-Vonk method. We expect that this study would be applicable to evaluate the crystallinity index of various cellulose materials with accuracy and reproducibility.

• 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.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.42 no.3
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• pp.297-302
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• 2016

In this study, we prepared liquid crystal emulsions composed of $C_{12-20}$ alkyl glucoside, $C_{14-22}$ alcohol, and behenyl alcohol and performed structure analysis using various analytical equipment. First, as an important characteristic of liquid crystal emulsions, maltese cross patterns and multi-layer structure were observed by a polarized microscope and cryo-SEM. Also, formation of liquid crystal phase was confirmed by DSC and multi-layer lamellar structure having an interlayer spacing approximately $305{\AA}$ was confirmed by small angle x-ray scattering (SAXS). The alkyl chain arrangement formed orthorhombic structure of a lamellar structure of the liquid crystal emulsion was confirmed by wide angle x-ray scattering (WAXS). These results suggest that information on the various physical properties obtained through the research of liquid crystal emulsion structure is expected to be widely used in cosmetics development in the future.

• Elastomers and Composites
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• v.48 no.1
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• pp.85-91
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• 2013

In this study, we synthesized a terpolymer consisting of ethylene, 1-hexene, and styrenic monomer using a metallocene catalyst and cocatalyst ststem. The styrenic monomers empolyed as the third monomer were styrene, p-methylstyrene, and 4-tert-butylstyrene. The structure and composition of the terpolymers were characterized using $^{13}C$ NMR and $^1H$ NMR. Catalytic activity, polymer yield, molecular weight and molecular weight distribution of the terpolymers were analyzed. We also determined the glass transition temperature(Tg), crystallinity and thermal properties of the terpolymers by DMA, WAXS and TGA.

• Journal of the Korean Wood Science and Technology
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• v.34 no.3
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• pp.38-45
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• 2006

The main objective of this study is the improvement of the interfacial adhesion of RHF-polypropylene (PP) bio-composites through NaOH and acetic acid treated RHF. After manufacturing of untreated and NaOH and acetic acid treated RHF filled PP bio-composites, the effect on interfacial adhesion of bio-composites was investigated. Tensile strength of the bio-composites made from treated RHF with NaOH and acetic acid was higher than that of the untreated bio-composites. The RHF surface before and after NaOH and acetic acid treatment was clearly confirmed by scanning electron microscopy (SEM) micrograph. It was found that both treatments result in a removal of impurity materials of RHF surface by SEM micrographs. The chemical structures of untreated and NaOH and acetic acid treated RHF were confirmed by fourier transform infrared (FTIR). The crystallization structure and crystallinity of non-treated, NaOH and acetic acid treated RHF were investigated by wide-angle X-ray scattering (WAXS).

• Bulletin of the Korean Chemical Society
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• v.17 no.1
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• pp.11-15
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• 1996

A series of poly(1,4-phenylene terephthalates) with pendant NLO chromophores was prepared by the solution polycondensation of 2,5-NLO chromophore substituted terephthalic acid with hydroquinone. The polymers obtained gave satisfactory NMR and elemental analysis results when taking into account their expected structures and the inherent viscosity value proved the polymeric character of all polymers. DSC, optical polarizing microscopy and WAXS studies revealed that none of these polymers exhibited liquid crystalline mesophases. Preliminary results on NLO properties of these polymers showed a surprisingly large second harmonic signal relative to a Y-cut quartz plate.

• Membrane Journal
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• v.18 no.2
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• pp.132-137
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• 2008

Nanofiltration membranes were prepared based on coating a sulfonated comb-like copolymer layer on top of a poly(vinylidene fluoride) (PVDF) support. The comb-like copolymer comprising poly(vinyl chloride) backbone and poly(styrene sulfonic acid) side chains, i.e. PVC-g-PSSA was synthesized by atom transfer radical polymerization (ATRP) using direct initiation of the secondary chlorines of PVC. The successful synthesis of graft copolymers were confirmed by nuclear magnetic resonance ($^1H$-NMR), FT-IR spectroscopy and wide angle X-ray scattering (WAXS). Composite nanofiltration membranes consisting PVC-g-PSSA as a top layer exhibited the increase of both rejections and solution flux with increasing PSSA concentration. This performance enhancement is presumably due to the increase of SO3H groups and membrane hydrophilicity. The rejections of composite membranes containing 71 wt% of PSSA were 88% for $Na_2SO_4$ and 33% for NaCl, and the solution flux were 26 and $34L/m^2h$, respectively, at 0.3 MPa pressure.

• Proceedings of the Polymer Society of Korea Conference
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• 2006.10a
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• pp.371-372
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• 2006

Poly(${\varepsilon}-caprolactone$) (PCL) is a highly crystalline polymer that is miscible with several amorphous polymers including chlorinated polyether, poly(vinylchloride), poly(hydroxyether) and Bisphenol A polycarbonate. The crystallization behavior of miscible blend of amorphous/crystalline polymers has widely been studied. Generally a depression of the crystallization ability has been found with addition of amorphous component because of the reduction of chain mobility, the change of free energy of nucleation as a result of a specific interaction, and so on [1]. In this work, for the first time, the blend of PCL and copolymer of polyurethane containing polycaprolactone as a soft segment is considered. The structural similarity of TPU soft segment with PCL affects on formation of the miscible component and crystallization behavior of PCL in the blend. This has been studied using differential scanning calorimetry (DSC) and Wide-angle X-ray Scattering (WAXS).