• Title/Summary/Keyword: SAXS(Small angle X-ray scattering)

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Structural Changes of Biodegradable Poly(tetramethylene succinate) on Hydrolysis

  • Shin, Jick-Soo;Yoo, Eui-Sang;Im, Seung-Soon;Song, Hyun-Hoon
    • Macromolecular Research
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    • v.9 no.4
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    • pp.210-219
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    • 2001
  • Quenched and slow cooled as well as isothermally crystallized poly(tetramethylene succinate)(PTMS) films at two different temperatures were prepared. In the process of hydrolysis of the four specimens, structural changes such as the crystallinity, crystal size distribution, lattice parameter, lamellar thickness, long period and surface morphology were investigated by using wide and small angle X-ray scattering (WAXS and SAXS), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). The hydrolytic degradation of quenched film was faster than that of slow cooled and isothermally crystallized films. The film crystallized at 100$\^{C}$ exhibited extensive micro voids and thus showed faster degradation than that crystallized at 75$\^{C}$, demonstrating surface morphology is another important factor to govern degradation rate. The crystallinity of the specimen increased by 5-10% and long period decreased after hydrolysis for 20 days. At the initial stage of degradation, the lamellar thickness of quenched film rather increased, while that of slow cooled and isothermally crystallized films decreased. The hydrolytic degradation preferentially occurred in the amorphous region. The hydrolytic degradation in crystal lamellae are mainly at the crystal surfaces.

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Effects of Physico-chemical Factors of Sol on the Degree of Preferred Orientation in $Pb(Mg, Zn)_{1/3}Nb_{2/3}O_3$ Thin Films (Sol의 물리화학적 변수들이 $Pb(Mg, Zn)_{1/3}Nb_{2/3}O_3$ 박막의 우선 배향성에 미치는 효과)

  • 조문규;장현명;김광수
    • Journal of the Korean Ceramic Society
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    • v.32 no.3
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    • pp.305-312
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    • 1995
  • Thin films of Pb(Mg, Zn)1/3Nb2/3O3 were fabricated by spin coating the Pb-Mg-Zn-Nb-O complex alkoxide sols on(111) Pt-coated MgO (100) planes. It was observed that the content of H2O and the rheological characteristics of sol greatly influenced the orientation of perovskite grains after thin-film formation. A strong preferential orientation of (100)-type planes of the perovskite grains was obtained for the sol aged for 15 days with the molar ratio of H2O to total metal alkoxides=2. As small angle X-ray scattering experiment in the Porod region was performed to correlate the observed preferential orientation with the network structure of precursors at various stage of aging. It was shown that the degree of branching of the Pb-Mg-Zn-Nb-O precursor chain had a direct effect on the preferred oreintation, and weakly branched precursor systems led to highly oriented grains after thin-film formation.

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Synthesis and Characterization of Cu2+-Perfluorophthalocyanine Incorporated SBA15

  • Oh, Mi-Ok;Park, Sung Soo;Ha, Chang-Sik
    • Journal of Adhesion and Interface
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    • v.7 no.3
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    • pp.10-15
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    • 2006
  • After anchoring 3-(2-aminoethylamino)propyltriethoxysilane (APTES) onto the surfaces of the channels within ordered mesoporous silica, SBA-15, we dispersed $Cu^{2+}$-perfluorophthalocyanine into the modified SBA-15 channels. From small-angle X-ray scattering (SAXS) patterns and transmission electron microscopy (TEM) images, we confirmed that both the calcined and $Cu^{2+}$-perfluorophthalocyanine-incorporated SBA-15 samples possessed ordered periodic structures and hexagonal symmetry lattices (p6mm). The value of the $d_{100}$ spacing was decreased after the incorporation of $Cu^{2+}$-perfluorophthalocyanine into the modified SBA-15 channels. We used FTIR and UV-Vis spectroscopy and thermogravimetric analysis (TGA) to characterize both the modified SBA-15 and the $Cu^{2+}$-perfluorophthalocyanine-incorporated SBA-15 samples. From scanning electron microscopy (SEM) images and $N_2$ sorption measurements, we found that the $Cu^{2+}$-perfluorophthalocyanine units were incorporated within the modified SBA-15 channels, rather than on the external surfaces of the modified SBA-15 channels.

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Development of Lamella Morphology in Poly(ethylene terephthalate)/Polycarbonate Blends

  • Lee, Jong-Kwan;Im, Jeong-Eon;Lee, Kwang-Hee
    • Macromolecular Research
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    • v.12 no.2
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    • pp.172-177
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    • 2004
  • We have studied the lamella-level morphology of poly(ethylene terephthalate) (PET)/polycarbonate (PC) blends using small-angle X-ray scattering (SAXS). Measurements were made as a function of the holding time in the melt. We determined the morphological parameters at the lamellar level by correlation function analysis of the SAXS data. An increased amorphous layer thickness was identified in the blend, indicating that some PC was incorporated into the interlamellar regions of PET during crystallization. The blend also exhibits a larger lamella crystalline thickness (l$\sub$c/) than that of pure PET. A possible reason for the increase in l$\sub$c/ is that the inclusion of the PC molecules in the interlamellar regions causes an increase in the surface free energy of folding. At the early stage of isothermal crystallization, we observed a rapid drop in the value of l$\sub$c/ in the blend; this finding indicates that a relatively large fraction of secondary crystals form during the primary crystallization. In contrast, the value of l$\sub$c/ for the sample that underwent a prolonged holding time increased with time in the secondary crystallization-dominant regime; this observation suggests that the disruption of chain periodicity, which results from transesterification between the two polymers, favors the development of fringed micellar crystals that have larger values of l$\sub$c/ rather than the development of normal chain-folded crystals.

Characteristics of composite membranes containing ionic liquid and acid for anhydrous high temperature PEFCs (무가습 고온 PEFC용 이온성 액체 및 산이 함유된 복합막의 특성)

  • Baek, Ji-Suk;Park, Jin-Soo;Park, Seung-Hee;Yang, Tae-Hyun;Park, Gu-Gon;Yim, Sung-Dae;Kim, Chang-Soo;Shul, Young-Gun
    • 한국신재생에너지학회:학술대회논문집
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    • 2009.06a
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    • pp.378-378
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    • 2009
  • The ionic liquid-based sulfonated hydrocarbon composite membranes was prepared for use in anhydrous high temperature-polymer electrolyte fuel cells (HT-PEFCs). Ionic liquid behaves like water in the composite membranes under anhydrous condition. However the composite membranes show a low conductivity and high gas permeability as the content of ionic liquid increases due to its high viscosity and content of ionic liquid, respectively. Hence, in order to enhance the proton conductivity and to reduce the gas permeability of the composite membranes with low content of ionic liquids, the acid containing a common ion of ionic liquid was added to the composite membranes. The characterization of composite membranes was carried out using small-angle X-ray scattering (SAXS), thermogravimetric analyzer (TGA) and impedance spectroscopy. As a result, the composite membranes containing acid showed higher proton conductivity than those with no acid under the un-humidified condition due to a decrease in viscosity. In addition, the proton conductivity of composite membranes increased with increasing mole concentration of acid.

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Characteristics of Poly(vinyl phenol) Ionomers Neutralized by LiOH and Their Miscibility with Poly(methyl methacrylate) (Li으로 중화된 폴리비닐페놀 이오노머의 특성 및 폴리메틸메타크릴레이트와의 혼화성)

  • 노진영;김진환
    • Polymer(Korea)
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    • v.24 no.6
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    • pp.886-892
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    • 2000
  • Poly(4-vinyl phenol) (PVPh) was neutralized by LiOH and PVPh ionomers (PVPh-Li) with different Li neutralization extents were synthesized. The variation in $T_{g}$ with Li neutralization was determined by DSC and the results show that the $T_{g}$ increases by 3.$8^{\circ}C$ per Li mol%. When comparing this result with the 3.$2^{\circ}C$ per Na mol% reported for poly (styrene-co-hydroxy styrene), the greater value for PVPh-Li may be due to a strong interaction between unneutralized free -OH and -OLi produced. No distinct small angle X-ray scattering (SAXS) peak was observed for these PVPh ionomers in bulk. In the 50/50 blend of PVPh-Li with PVPh, the miscibile blend was obtained when the Li neutralization in PVPh-Li was 10 mol%. On the contrary, the 50/50 PVPh-Li/PMMA was immiscible when the Li neutralization was 5 mol%. It can be concluded that, even if the starting blend is miscible owing to hydrogen bonding, the miscibility of blend becomes diminished by introducing small amount of ion groups into one of the constituent polymers and the blend can be immiscible as long as any new strong intermolecular ion-dipole interaction is not generated.

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Phase Behavior Study of Fatty Acid Potassium Cream Soaps (지방산 칼륨 Cream Soaps 의 상거동 연구)

  • Noh, Min Joo;Yeo, Hye Lim;Lee, Ji Hyun;Park, Myeong Sam;Lee, Jun Bae;Yoon, Moung Seok
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.48 no.1
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    • pp.55-64
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    • 2022
  • The potassium cream soap with fatty acid called cleaning foam has a crystal gel structure, and unlike an emulsion system, it is weak to shear stress and shows characteristics that are easily separated under high temperature storage conditions. The crystal gel structure of cleansing foams is significantly influenced by the nature and proportion of fatty acids, degree of neutralization, and the nature and proportion of polyols. In order to investigate the effect of these parameters on the crystal gel structure, a ternary system consisting of water/KOH/fatty acid was investigated in this study. The investigation of differential scanning calorimeter (DSC) revealed that the eutectic point was found at the ratio of myristic acid (MA) : stearic acid (SA) = 3 : 1 and ternary systems were the most stable at the eutectic point. However, the increase in fatty acid content had little effect on stability. On the basis of viscosity and polarized optical microscopy (POM) measurements, the optimum degree of neutralization was found to be about 75%. The system was stable when the melting point (Tm) of the ternary system was higher than the storage temperature and the crystal phase was transferred to lamellar gel phase, but the increase in fatty acid content had little effect on stability. The addition of polyols to the ternary system played an important role in changing the Tm and causing phase transition. The structure of the cleansing foams were confirmed through cryogenic scanning electron microscope (Cryo-SEM), small and wide angle X-ray scattering (SAXS and WAXS) analysis. Since butylene glycol (BG), propylene glycol (PG), and dipropylene glycol (DPG) lowered the Tm and hindered the lamellar gel formation, they were unsuitable for the formation of stable cleansing foam. In contrast, glycerin, PEG-400, and sorbitol increased the Tm, and facilitated the formation of lamellar gel phase, which led to a stable ternary system. Glycerin was found to be the most optimal agent to prepare a cleansing foam with enhanced stability.