• 제목/요약/키워드: small-angle light scattering

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SALS를 이용한 고분자용액의 상전환 기구에 관한 연구 : C1-C4 알콜의 첨가에 따른 상분리 거동에 미치는 효과와 투과 특성 (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)

  • Kang, Jong-Seok;Lee, Young-Moo
    • 한국막학회:학술대회논문집
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    • 한국막학회 2002년도 춘계 총회 및 학술발표회
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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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스피노달 분해와 기핵성장에 따른 상분리 과정의 광산란 패턴의 관찰 (The Observation of Scattering Patterns During Membrane Formation: Spinodal Decomposition and Nucleation Growth)

  • 강종석;허훈;이영무
    • 멤브레인
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    • 제12권2호
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    • pp.97-106
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    • 2002
  • Polysulfone (PSf/NMP/alcohol 용액과 chlorinated poly(vinyl chloride) (CPVC)/THF/Alcohol 용액에 대한 광산란 패턴을 SALS (Small angle light scattering)와 FE-SEM (field emission scanning electron microscope)을 이용하여 조사하였다. PSf 용액에서는 시간에 따라 q값의 최대 산란 강도를 보이는 광산란 거동을 나타내어 스피노달 (SD) 상분리 거동을 나타내는 반면, CPVC 용액에서는 q값이 증가함에 따라 광산란 강도가 줄어드는 핵성장 (NG) 거동을 나타냈다. 각 고분자 용액에서 상분리 중반과 후반부에서 비용매 첨가제로 사용된 알코올의 탄소수가 증가할수록 농도분극의 증가율은 줄어들었다. 또한, SD에서의 초반부의 시간에 따른 산란 강도는 비용매 첨가제의 종류에 무관하게 Cahn의 건형 이론에 잘 부합되었다. 또한, SALS 장치로 얻어진 기공크기와 전자현미경으로 얻어진 영역 크기는 상호간에 비교되었다. 20PSf/70NMP/10n-butano1 (w/w%) 용액에 대한 산란 패턴은 초기 상분리 거동에서부터 후기 거동까지 매우 선명하게 관측되었고, 초반, 중반, 그리고 후반부에 대한 SD에 대한 이론적 결과와 잘 일치하였다. 최고의 산란강도를 나타낸 각도의 크기는 n-butanol>n-propanol>methanol>no alcohol 순으로 관찰되었으며, 이 순서로 최종 형성된 막 단면의 기공 크기가 감소되는 것으로 조사되었다.

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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    • 제6권1호
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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.

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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    • 제14권5호
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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.

SAXS와 AFM에 의한 HF-용액내 양극 에칭에 의해 제조된 기공성 실리콘의 구조연구 (SAXS and AFM Study on Porous Silicon Prepared by Anodic Etching in HF-based Solution)

  • 김유진;김화중
    • 한국전기전자재료학회논문지
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    • 제17권11호
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    • pp.1218-1223
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    • 2004
  • Porous silicon materials have been shown to have bright prospects for applications in light emitting, solar cell, as well as light- and chemical-sensing devices. In this report, structures of porous silicon prepared by anodic etching in HF-based solution with various etching times were studied in detail by Atomic Force Microscopy and Small Angle X -ray Scattering technique using the high energy beam line at Pohang Light Source in Korea. The results showed the coexistence of the various pores with nanometer and submicrometer scales. For nanameter size pores, the mixed ones with two different shapes were identified: the larger ones in cylindrical shape and the smaller ones in spherical shape. Volume fractions of the cylindrical and the spherical pores were about equal and remained unchanged at all etching times investigated. On the whole uniform values of the specific surface area and of the size parameters of the pores were observed except for the larger specific surface area for the sample with the short etching time. The results implies that etching process causes the inner surfaces to become smoother while new pores are being generated. In all SAXS data at large Q vectors, Porod slope of -4 was observed, which supports the fact that the pores have smooth surfaces.

Morphology Development in a Range of Nanometer to Micrometer in Sulfonated Poly(ethylene terephthalate) Ionomer

  • Lee, Chang-Hyung;Inoue, Takashi;Nah, Jae-Woon
    • Bulletin of the Korean Chemical Society
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    • 제23권4호
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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.

Phase Behavior of a PEO-PPO-PEO Triblock Copolymer in Aqueous Solutions: Two Gelation Mechanisms

  • Park, Moon-Jeong;Kookheon Char;Kim, Hong-Doo;Lee, Chang-Hee;Seong, Baek-Seok;Han, Young-Soo
    • Macromolecular Research
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    • 제10권6호
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    • pp.325-331
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    • 2002
  • Phase behavior of a PEO-PPO-PEO (Pluronic P103) triblock copolymer in water is investigated using small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and rheology. Pluronic P103 shows apparent two gel states in different temperature regions. The first sol-to-gel transition at a lower temperature (i.e., the hard gel I state) turns out to be the hexagonal microphase as evidenced by the combined SANS and SAXS and the frequency dependence of both G′ and G" in rheology. In contrast to the hard gel I, the second sol-to-gel transition (i. e., the hard gel II state) at a higher temperature represents the block copolymer micelles in somewhat disordered state rather than the ordered state seen in the hard gel I. Moreover, turbidity change depending only on the temperature with four distinct regions is observed and the large aggregates with size larger than 5,000 nm are detected with DLS in the turbid solution region. Based upon the present study, two different gelation mechanisms for aqueous PEO-PPO-PEO triblock copolymer solutions are proposed.

PHASE VARIATION IN DOPPLER SIGNAL FOR VARIOUS OPTICAL PARAMETERS

  • Son, Jung-Young;Kim, Myung-Sik;Oh, Myung-Kwan
    • 대한전기학회:학술대회논문집
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    • 대한전기학회 1989년도 하계종합학술대회 논문집
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    • pp.629-632
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    • 1989
  • The scattered light intensity from a spherical particle passing through the cross-over region of two coherent laser beams, varies periodically. Photodetection of this light beams produces a periodic signal of varying amplitude. The phase of the signal varies with the particle size and refractive index, the beam crossing angle and wavelength, and the position and size of the scattered ligth collecting aperture. In this paper the phase variation with respect to the particle absorptive index of retraction, collecting lens size and beam crossing angle is calculated using both Mie scattering theory and reflection theory. The two theories show good agreement in phase predictions, especially for large absorptive indices and for small collection lenses. Both theories predict phase to be inversely proportional to the beam crossing angle.

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Spherulitic Morphologies of Poly(ethylene terephthalate), Poly(ethylene 2,6-naphthalate), and Their Blend

  • Lee, Jong-Kwan;Lee, Kwang-Hee;Jin, Byung-Suk
    • Macromolecular Research
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    • 제10권1호
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    • pp.44-48
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    • 2002
  • The supermolecular structures of poly(ethylene terephthalate) (PET), poly(ethylene 2,6-naphthalate) (PEN), and their blend were investigated with optical microscopy and small angle light scattering. With increasing the crystallization temperature, incomplete spherulitic texture was developed for the PET samples. At a high crystallization temperature of 220 $^{\circ}C$, the light scattering pattern represented a random collection of uncorrelated lamellae. The general morphological appearances for the PEN samples were similar to that of the PET. A notable feature was that the spherulites of the PEN formed at 200 $^{\circ}C$ showed regular concentric bands arising from a regular twist in the radiating lamellae. The spherulitic morphology of the PET/PEN blend was largely influenced by the changes of the sequence distribution in polymer chains determined by the level of transesterifcation. The increased sequential irregularity in the polymer chains via transesterification caused a morphological transition from a regular folded crystallite to a tilted lamellar crystallite.