• Title/Summary/Keyword: small angle light scattering (SALS)

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The Observation of Scattering Patterns During Membrane Formation: Spinodal Decomposition and Nucleation Growth (스피노달 분해와 기핵성장에 따른 상분리 과정의 광산란 패턴의 관찰)

  • Kang, Jong-Seok;Huh, Hoon;Lee, Young-Moo
    • Membrane Journal
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    • v.12 no.2
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    • pp.97-106
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    • 2002
  • Small angle light scattering (SALS) and field emission scanning electron microscope (FE-SEM) have been used to investigate the light scattering patterns with time evolved during water vapor quenching (relative humidity of 53 (${\pm}3)%$ at $26^{\circ}C$ of polysulfone (PSf)/NMP/Alcohol and chlorinated poly(vinyl chloride) (CPVC)/THF/Alcohol, respective1y. Time dependence of the position of the light scattering maximum was observed at PSf dope solutions, confirming spinodal decomposition (SD), while CPVC dope solutions showed a decreased scattered light intensity with an increased q-value, indicating nucleation & growth (NG). For the each system, domain growth rate in the intermediate and late stage of phase separation decreased with increasing the number of carbon of alcohol used as additive (non-solvent). Also, in the early stage for SD, the scattering intensity with time was in accordance with Cahn's linear theory of spinodal decomposition, regardless of types of non-solvent additive. Also, the size scales obtained by SALS were mutually compared to domain sizes gained by FE-SEM measurement. These observations of scattering pattern were much clearly observed for the 20PSf/70NMP/10n-butanol (w/w%) and agreed with the theoretical predictions for scattering patterns of each stage like the early, the intermediate, and the late stage of SD type phase separation. As the scattering maximum was observed at the larger angles (larger q) in the order of n-butanol > n-propanol > methanol > no alcohol, the pore size of final morphology decreased.

SALS Study on Transcrystallization and Fiber Orientation in Glass Fiber/Polypropylene Composites

  • Na, Kun;Park, Han-Soo;Won, Hong-Youn;Lee, Jong-Kwan;Lee, Kwang-Hee;Nam, Joo-Young;Jin, Byung-Suk
    • Macromolecular Research
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    • v.14 no.5
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    • pp.499-503
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    • 2006
  • This report presents a new technical approach for evaluating the fiber orientation of composites using small-angle light scattering (SALS). Glass fiber (GF)/polypropylene (PP) composites with different fiber orientations were prepared by drawing compression-molded specimens. The drawn samples were remelted and then annealed at $150^{\circ}C$ in order to induce a crystalline structure on the fiber surface, and then underwent SALS analysis. The samples showed a combination of circular and streak patterns. The model calculations demonstrated that the number of nuclei on the fiber surface and the thickness of the transcrystalline layer affected the sharpness and intensity of the streak pattern. In addition, the azimuthal angle of the streak pattern was found to be dependent on the direction of the transcrystalline layer, which correlated with the fiber direction. This correlation suggests that the fiber orientation in the composites can be easily evaluated using SALS.

The Observation of Nucleation & Growth during Water Vapor Induced Phase Inversion of Chlorinated Poly(vinyl chloride) Solution using SALS

  • Jang, Jae Young;Lee, Young Moo;Kang, Jong Seok
    • Korean Membrane Journal
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    • v.6 no.1
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    • pp.61-69
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    • 2004
  • Small angle light scattering (SALS) and field emission scanning electron microscope (FE-SEM) have been used to investigate the effects of alcohol on phase separation of chlorinated poly(vinyl chloride) (CPVC)/tetrahydrofuran (THF)/alcohol (9/61/30 wt%) solution during water vapor induced phase separation. A typical scattering pattern of nucleation & growth (NG) was observed for all casting solutions of CPVC/THF/alcohol. In the case of the phase separation of CPVC dope solution containing 30 wt% ethanol or n-propanol, the demixing with NG was observed to be heterogeneous. Meanwhile, the phase separation of CPVC dope solution with 30 wt% n-butanol was found to be predominantly homogeneous NG. Although the different phase separation behavior of NG was observed with types of alcohol additives, the resultant surface morphology had no remarkable differences. That is, even though the NG process by water vapor is either homogeneous or heterogeneous, this difference does not play a main role on the final surface morphology. However, it was estimated from the result of hydraulic flux that the phase separation by homogeneous NG provided the membrane geometry with lower resistance in comparison with that by heterogeneous one.

The study of phase inversion of polymer solutions using small angle light scattering (SALS): The effect of addition of alcohol (C1-C4) on phase separation behavior and hydraulic permeation (SALS를 이용한 고분자용액의 상전환 기구에 관한 연구 : C1-C4 알콜의 첨가에 따른 상분리 거동에 미치는 효과와 투과 특성)

  • Kang, Jong-Seok;Lee, Young-Moo
    • Proceedings of the Membrane Society of Korea Conference
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    • 2002.05a
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    • pp.81-85
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    • 2002
  • Small angle light scattering and field emission scanning electron microscope have been used to quantify the kinetics of liquid-liquid separation behavior during water vapor(RH52%[$\pm$3%] at 27$^{\circ}C$) quenching (non-solvent induced phase separation, NIPS) of polysulfone/NMP/Alcohol and CPVC/THF/Alcohol, respectively. Time dependence of the position of the light scattering maximum was observed at polysufone dope solutions, confirming spinodal secomposition (SD). while CPVC dope solutions showed a decreased scattered light intensity with a increased q-valuel, indicating nucleation & growth (NG). For the each system, domain growth rate in the intermediate and late stage of phase separation decreased with increasing the number of carbon of alcohol used as additive (non-solvent). Also, in the early stage for SD, the scattering intensity with time was in accordance with Cahns linear theory of spinodal decomposition,[1-3] regardless of types of non-solvent additive.

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THERMALLY INDUCED PHASE SEPARATION IN TERNARY POLYMER SOLUTION

  • Jung, Bum-Suk;Kang, Yong-Soo;Jones, Richard-A.L.
    • Proceedings of the Membrane Society of Korea Conference
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    • 1999.07a
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    • pp.79-82
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    • 1999
  • Using Small Angle Light Scattering (SALS), the effect of quench depth on the kinetics of phase separation for ternary solution blends was investigated. The system was composed of two polymers (polystyrene and polybutadiene) and a solvent (toluene). The analyses of the early stage of phase separation were based of the Cahn-Hilliard theory [1,5]. Apparent diffusion coefficients and the fastest mode of fluctuations were evaluated, when quench depth of the system were varied near the critical composition of polymer. In the late stage of phase separation, the domain growth showed a power law with the 1/3 exponent, i.e. $q_m(t)~t^{-1/3}$. For comparison between real images and scattering profiles with time, the image of phase domains with time were obtained by using Laser Confocal Scanning Microscopy (LSCM).

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Morphology and Crystallization in Mixtures of Poly(methyl methacrylate)-Poly(pentafluorostyrene)-Poly(methyl methacrylate) Triblock Copolymer and Poly(vinylidene fluoride)

  • Kim, Geon-Seok;Kang, Min-Sung;Choi, Mi-Ju;Kwon, Yong-Ku;Lee, Kwang-Hee
    • Macromolecular Research
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    • v.17 no.10
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    • pp.757-762
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    • 2009
  • The micro domain structures and crystallization behavior of the binary blends of poly(methyl methacrylate)-b-poly(pentafluorostyrene)-b-poly(methyl methacrylate) (PMMA-PPFS-PMMA) triblock copolymer with a low molecular weight poly(vinylidene fluoride) (PVDF) were investigated by small-angle X-ray scattering (SAXS), small-angle light scattering (SALS), transmission electron microscopy (TEM), optical microscopy, and differential scanning calorimetry (DSC). A symmetric, PMMA-PPFS-PMMA triblock copolymer with a PPFS weight fraction of 33% was blended with PVDF in N,N-dimethylacetamide (DMAc). In the wide range of PVDF concentration between 10.0 and 30.0 wt%, PVDF was completely incorporated within the PMMA micro domains of PMMA-PPFS-PMMA without further phase separation on a micrometer scale. The addition of PVDF altered the phase morphology of PMMA-PPFS-PMMA from well-defined lamellar to disordered. The crystallization of PVDF significantly disturbed the domain structure of PMMA-PPFS-PMMA in the blends, resulting in a poorly-ordered morphology. PVDF displayed unique crystallization behavior as a result of the space constraints imposed by the domain structure of PMMA-PPFS-PMMA. The pre-existing microdomain structures restricted the lamellar orientation and favored a random arrangement of lamellar crystallites.

Miscibility and Properties of Ethyl-Branched Polyethylene/Ethylene-Propylene Rubber Blends (II) (에틸 가지화된 폴리에틸렌과 에틸렌-프로필렌 고무 블렌드의 혼화성과 물성(II))

  • Cho, Ur-Ryong
    • Elastomers and Composites
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    • v.37 no.2
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    • pp.79-85
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    • 2002
  • Ethyl-branched polyethylene [PE(2)] containing 2mole% ethyl branch and three ethylene-propylene rubbers (EPR's) having the same ethylene(E)-propylene(P) molar ratio(E/P=50/50) with different stereoregularity, that is, random EPR (r-EPR), alternating-EPR (alt-EPR) and isotactic-alternating-EPR (iso-alt-EPR) were mixed for the investigation or their properties depending on the stereoregularity. Crystallinity of the prepared blends decreased with increasing content of amorphous EPR because of a decrease in both the degree of annealing and kinetics of diffusion of the crystallizable polymer content. With blend composition, crystallinity was reduced with the stereoregularity in EPR. The thermodynamic interaction parameter(x) for the three blend systems approximately equals to zero near the melting point. These systems were determined to be miscible on a molecular scale near or above the crystalline melting point or the crystalline PE(2). From the measurement of $T_m$ vs. $T_c$, the behavior of PE(2) is mainly due to a diluent effect of EPR component. The spherulite size measured by small angle light scattering (SALS) technique depended upon blend composition, and stereoregularity of EPR. The size of spherulite was enlarged with the content of rubbery EPR and the decrease of stereoregularity in EPR.