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

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Effects of Pentanol on the Rheology of Lecithin/LiCl Oranogel (Lecithin/LiCl 유기젤의 펜탄올 영향에 대한 유변학적 연구)

  • Kim, Min-Gook;Chu, Eun-Ae;Lee, Hee-Young
    • Applied Chemistry for Engineering
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    • v.32 no.6
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    • pp.679-683
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    • 2021
  • Lecithin, a zwitterionic phospholipid, forms spherical reverse micelles in nonpolar organic solvents such as decane. The addition of monovalent ions like lithium chloride (LiCl) to lecithin organosols induces the transformation of organosols into organogels due to the entanglement of reverse cylindrical micelles. In this study, we investigate the effect of pentanol acting as co-surfactant on rheological properties of lecithin/LiCl mixtures. From rheological studies, we find that the viscosity and elastic property of organogels decreased upon the addition of pentanol to organogels. The decrease in viscosity and elastic property can be attributed to the shortening of reverse cylindrical micelles confirmed by small angle X-ray scattering (SAXS).

Investigation of Rheological Properties of Lecithin/D-sorbitol/Water Mixtures (레시틴/디솔비톨/물 혼합물의 유변학적 성질 연구)

  • Eun-Ae Chu;Na-Hyeon Kim;Min-Seok Kang;Yeong-Min Lee;Hee-Young Lee
    • Applied Chemistry for Engineering
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    • v.34 no.3
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    • pp.247-251
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    • 2023
  • Lecithin can self-assemble into reverse spherical micelles in organic solvents due to its amphiphilic properties. With additives such as D-sorbitol and water, the reverse spherical micelles are transformed into reverse cylindrical micelles by the morphology change of lecithin molecules. In this study, the rheological properties of lecithin/D-sorbitol/water mixtures were investigated. In addition, the small angle X-ray scattering (SAXS) technique was used to examine the shape and size of the formed nanostructures related to their rheological properties. Such mixtures are expected to be used in drug delivery and oleogels because of their high viscosity and viscoelastic behavior.

Vacuum Carbonization of Nanometer Tungsten Powder with Carbon Black

  • Luo, Ji;Lin, Tao;Guo, Zhi-meng;Jia, Chengchang
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2006.09a
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    • pp.442-443
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    • 2006
  • Vacuum carbonization of nanometer tungsten powder was investigated in a simple designed apparatus. An X-Y recorder was used to plot differential thermal analysis (DTA) curves to determine starting temperature of carbonization of four samples with different specific surface area. The product was detected by X-ray Diffraction (XRD) and small angle X-ray scattering (SAXS). The results show that finer tungsten powder has lower starting temperature of carbonization. Tungsten powder, which BET surface area is $32.97m^2/g$, is completely carbonized to tungsten carbide at $1050^{\circ}C$, although the starting temperature is $865^{\circ}C$. Particle grows sharply before carbonization.

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Synthesis and Characterization of Nanocomposite Films Consisting of Vanadium Oxide and Microphase-separated Graft Copolymer

  • Choi, Jin-Kyu;Kim, Yong-Woo;Koh, Joo-Hwan;Kim, Jong-Hak;Mayes, Anne M.
    • Macromolecular Research
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    • v.15 no.6
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    • pp.553-559
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    • 2007
  • Nanocomposite films were prepared by sol-gel synthesis from vanadium triisopropoxide with $poly((oxyethylene)_9$ methacrylate)-graft-poly(dimethyl siloxane), POEM-g-PDMS, producing in situ growth of vanadium oxide within the continuous ion-conducting POEM domains of micro phase-separated graft copolymer. The formation of vanadium oxide was confirmed by wide angle x-ray scattering (WAXS) and Fourier transform infrared (FT-IR) spectroscopy. Small angle x-ray scattering (SAXS) revealed the spatially-selective incorporation of vanadium oxide in the POEM domains. Upon the incorporation of vanadium oxide, the domain periodicity of the graft copolymer monotonously increased from 17.2 to 21.0 nm at a vanadium content 14 v%, above which it remained almost invariant. The selective interaction of vanadium oxide with POEM was further verified by differential scanning calorimetry (DSC) and FT-IR spectroscopy. The nanocomposite films exhibited excellent mechanical properties $(l0^{-5}-10^{-7}dyne/cm^2)$, mostly due to the confinement of vanadium oxide in the POEM chains as well as the interfaces created by the microphase separation of the graft copolymer.

Performance Test of 4Cl Beamline for Protein Solution Scattering at the PLS (용액상의 단백질 구조 분석을 위한 PLS 4Cl빔라인의 성능 테스트)

  • Yu Chung-Jong;Kim Jehan;Kim Kwang-Woo;Kim Ghyung-Hwa;Lee Heung-Soo;Ree Moonhor;Kim Kyung-Jin
    • Journal of the Korean Vacuum Society
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    • v.14 no.3
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    • pp.138-142
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    • 2005
  • We tested performance of the 4C1 beamline for analyzing structures of proteins in solution using small angle X-ray scattering (SAXS) at the Pohang Light Source(PLS). Structurally well-known proteins such as lysozyme and $Bcl-XL(\vartriangle TM/\vartriangle loop)$ were used for the study. Low resolution solution structures of lysozyme and $Bcl-XL(\vartriangle TM/\vartriangle loop)$ were obtained at a resolution of at least i.2 nm, and the structures were basically same as those calculated from the crystal structures of the proteins. We also used $Bcl-XL(\vartriangle TM/\vartriangle loop)$ with a long flexible loop attached [$Bcl-XL(\vartriangleTM))$] and obtained significantly different data from $Bcl-XL(\vartriangle TM/\vartriangle loop)$, although the electron density map of the loop is known to be invisible from the crystal structure of $Bcl-XL(\vartriangleTM))$. We confirm that SAXS experiment is a powerful tool for the structural study of proteins in solution and the 4Cl beamline at the PLS is well-equipped and suitable for the protein solution SAXS experiment.

Effect of A-Zeolite on the Crystallization Behavior of In-situ Polymerized Poly(ethylene terephthalate) (PET) Nanocomposites

  • Shin, Young-Hak;Lee, Wan-Duk;Im, Seung-Soon
    • 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.

Crystallization Behavior of Poly(ethylene terephthalate)/Ethylene-Methyl acrylate-Glycidyl methacrylate Copolymer Blend (폴리에틸렌테레프탈레이트/에틸렌-메틸아크릴레이트-글리시딜 메타크릴레이트 공중합물 블렌드의 결정화 거동)

  • 성상엽;이종관;이광희;진병석
    • Polymer(Korea)
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    • v.25 no.6
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    • pp.848-854
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    • 2001
  • The crystallization behavior of poly (ethylene terephthalate) (PET) /ethylene-methyl acrylate-glycidyl methacrylate copolymer (E-MeA-GMA) blend was studied. The extent of reaction and the reaction rate between PET and E-MeA-GMA were measured with torque rheometer, FT-IR and SEM. The effects of the grafting reaction on the crystallization behavior were investigated with DSC and time-resolved light scattering (TR-LS) techniques. The morphological change at the lamellar level was also examined by using a small angle X-ray scattering (SAXS) method.

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X-Ray Scattering Studies on Molecular Structures of Star and Dendritic Polymers

  • Jin, Sang-Woo;Jin, Kyeong-Sik;Yoon, Jin-Hwan;Heo, Kyu-Young;Kim, Je-Han;Kim, Kwang-Woo;Ree, Moon-Hor;Higashihara, Tomoya;Watanabe, Takumi;Hirao, Akira
    • Macromolecular Research
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    • v.16 no.8
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    • pp.686-694
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    • 2008
  • We studied the molecular shapes and structural characteristics of a 33-armed, star polystyrene (PS-33A) and two $3^{rd}$-generation, dendrimer-like, star-branched poly(methyl methacrylate)s with different architectures (pMMA-G3a and PMMA-3Gb) and 32 end-branches under good solvent and theta ($\Theta$) solvent conditions by using synchrotron small angle X-ray scattering (SAXS). The SAXS analyses were used to determine the structural details of the star PS and dendrimer-like, star-branched PMMA polymers. PS-33A had a fuzzy-spherical shape, whereas PMMA-G3a and PMMA-G3b had fuzzy-ellipsoidal shapes of similar size, despite their different chemical architectures. The star PS polymer's arms were more extended than those of linear polystyrene. Furthermore, the branches of the dendrimer-like, star-branched polymers were more extended than those of the star PS polymer, despite having almost the same number of branches as PS-33A. The differences between the internal chain structures of these materials was attributed to their different chemical architectures.

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.

Homopolymer Distribution in Polystyrene - Poly(methyl methacrylate) Diblock Copolymer (폴리스티렌-폴리(메틸 메타크릴레이트) 이종 블록 공중합체 내의 단일중합체 분포)

  • Hong, Sung-Ho;Lee, Eun-Ji;Song, Kwon-Bin;Lee, Kwang-Hee
    • Polymer(Korea)
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    • v.35 no.6
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    • pp.531-536
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    • 2011
  • Homopolymer distribution in block copolymer/homopolymer blends was investigated as a function of homopolymer concentration and homopolymer molecular weight. The deuterated poly(methyl methacrylate) or polystyrene was blended with a deuterated polystyrene-poly(methyl methacrylate) diblock copolymer up to a concentration of 20 wt%. Samples were characterized by small-angle X-ray scattering (SAXS), neutron reflectivity and transmission electron microscopy. The block copolymer with a thin-film geometry formed alternating lamellar microdomains oriented parallel to the substrate surface. By adding the homopolymer, the microdomain structure was significantly disturbed. As a consequence, a poorly ordered morphology appeared when the homopolymer concentration exceeded 15 wt%. Increasing the homopolymer concentration and/or the homopolymer molecular weight caused the microdomains to swell less uniformly, resulting in segregation of the homopolymer toward the middle of the microdomains.