• Title/Summary/Keyword: SAXS

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Thermal and Solid State Assembly Behavior of Amphiphilic Aliphatic Polyether Dendrons with Octadecyl Peripheries

  • Chung, Yeon-Wook;Lee, Byung-Ill;Cho, Byoung-Ki
    • Macromolecular Research
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    • v.16 no.2
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    • pp.113-119
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    • 2008
  • A series of amphiphilic dendrons n-18 (n: generation number, 18: octadecyl chain) based on an aliphatic polyether denderitic core and octadecyl peripheries were synthesized using a convergent dendron synthesis consisting of a Williamson etherification and hydroboration/oxidation reactions. This study investigated their thermal and self-assembling behavior in the solid state using differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) absorption spectroscopy, and small angle X-ray scattering (SAXS). DSC indicated that the melting transition and the corresponding heat of the fusion of the octadecyl chain decreased with each generation. FT-IR showed that the hydroxyl focal groups were hydrogen-bonded with one another in the solid state. DSC and FT-IR indicated microphase-separation between the hydrophilic dendritic cores and hydrophobic octadecyl peripheries. SAXS data analysis in the solid state suggested that the lower-generation dendrons 1-18 and 2-18 self-assemble into lamellar structures based upon a bilayered packing of octadecyl peripheries. In contrast, the analyzed data of higher-generation dendron 3-18 is consistent with 2-D oblique columnar structures, which presumably consist of elliptical cross sections. The data obtained could be rationalized by microphase-separation between the hydrophilic dendritic core and hydrophobic octadecyl peripheries, and the degree of interfacial curvature associated with dendron generation.

Ordering Kinetics of Triblock Copolymer/Low Molecular Weight Homopolymer Mixtures (삼중블록공중합체와 저분자량 단일중합체 혼합물의 미세상분리 동력학)

  • 차국헌
    • The Korean Journal of Rheology
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    • v.10 no.2
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    • pp.65-73
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    • 1998
  • 본연구에서는poystyrene-block-poly (ethlene-co-butylene)-block-polystyrene(SEBS) 삼중블록 공중합체와 저분자량 단일중합체인 Hercotac 1149 (H1149)의 70/30 (w/w) 혼합물 의 미세상분리와 그동력학을 유변물성 측정법과 SAXS 실험을 통하여 연구해 보았다. 먼저 혼합물의 미세상분리 온도를 유변물성 측정법과 SAXS 실험을 통해 각각구한 다음 샘플을 미세상분리 온도보다 높은 온도에서 그이하의 온도로 급냉시킨 후 유변물성과 산란강도의 사간에 따른 변화로부터 미세상분리 동력학에 대한 정보를 구하였다. 이렇게 얻어진 데이터 를 Avrami 형태의 핵생성 성장(NG) 메커니즘으로 해석해 보았는데 최대산란강도 Imax 뿐만 아니라 저장 점탄성계수 G'과 손실 점탄성계수 G"의 시간에 따른 변화를 잘 예측할수 있 었다. 한편 서로다른 두 time-resolved 실험으로부터 Avrami 플롯을 그려서 구해진 Avrami 변수들은 같은 급냉 깊이에서는 서로 잘 일치함을 확인하였다. 반감기는 급냉 깊이가 증가 함에 따라 점차 감소하는 경향을 보였는데 이는 급냉 깊이가 클수록 미세상분리가 더 빨리 진행되고 있음을 보여주는 것이다. 또한 Avrami 지수는 급냉 깊이가 증가함에 따라 3에서 4로 급격히 변했는데 이로부터 급냉 깊이가 작을 때에는 70/30 (w/w) SEBS/H1149 혼합물 의 미세상분리가 불균일 핵생성 성장 메커니즘에 따라 진행되고 급냉 깊이가 더 커지면 미 세상분리가 스피노달 상분리 메커니즘으로 변하고 있음을 예측할수 있었다.

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Liquid Crystal Emulsions Containing High Content Ceramides for Improved Skin Barrier Functions

  • Lee, Jun Bae;Noh, Minjoo;Kim, Su Ji;Jang, Jihui
    • Korea Journal of Cosmetic Science
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    • v.1 no.1
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    • pp.19-29
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    • 2019
  • In this work, we fabricated liquid crystal (LC) emulsions with fatty alcohol in order to stabilize high content ceramide in cosmetic formulation. We investigated the role of fatty alcohol and surfactant in the formation of higher order structure. As a result, we found that they play a crucial role to form higher order structure. SAXS study shows that ceramide can be incorporated up to 3% in cosmetic formulation with higher order structure and its stability was maintained up to 12 weeks at room temperature. According to WAXS study, the higher order structure can suppress the re-crystallization of ceramide in cosmetic formulation. Finally, we performed in vivo skin barrier recovery test for the damaged skin. LC emulsions with ceramide and O/W emulsions show significant effect in skin barrier recovery at D 1, D 2 and D 6 compared to the untreated condition. While only LC emulsions show significant skin recovery effect at D 14. We expect that LC emulsions are the promising skin carrier to stabilize ceramide and LC emulsions with ceramide can improve the skin barrier function.

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.

Current Status of the Synchrotron Small-Angle X-ray Scattering Station BL4C1 at the Pohang Accelerator Laboratory

  • Jorg Bolze;Kim, Jehan;Huang, Jung-Yun;Seungyu Rah;Youn, Hwa-Shik;Lee, Byeongdu;Shin, Tae-Joo;Moonhor Ree
    • Macromolecular Research
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    • v.10 no.1
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    • pp.2-12
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    • 2002
  • The small-angle X-ray scattering (SAXS) beamline BL4C1 at the 2.5 GeV storage ring of the Pohang Accelerator Laboratory (PAL) has been in its first you of operation since August 2000. During this first stage it could meet the basic requirements of the rapidly growing domestic SAXS user community, which has been carrying out measurements mainly on various polymer systems. The X-ray source is a bending magnet which produces white radiation with a critical energy of 5.5 keV. A synthetic double multilayer monochromator selects quasi-monochromatic radiation with a bandwidth of ca. 1.5%. This relatively low degree of monochromatization is sufficient for most SAXS measurements and allows a considerably higher flux at the sample as compared to monochromators using single crystals. Higher harmonics from the monochromator are rejected by reflection from a flat mirror, and a slit system is installed for collimation. A charge-coupled device (CCD) system, two one-dimensional photodiode arrays (PDA) and imaging plates (IP) are available its detectors. The overall performance of the beamline optics and of the detector systems has been checked using various standard samples. While the CCD and PDA detectors are well-suited for diffraction measurements, they give unsatisfactory data from weakly scattering samples, due to their high intrinsic noise. By using the IP system smooth scattering curves could be obtained in a wide dynamic range. In the second stage, stating from August 2001, the beamline will be upgraded with additional slits, focusing optics and gas-filled proportional detectors.

중성자 산란을 이용한 나노기공 측정

  • 최성민;이지환;조성민
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2002.11a
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    • pp.51-51
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    • 2002
  • 나노기공물질은 특정 기반물질(matrix) 내부에 대략 나노미터크기의 기공을 함유하고 있는 물질이며 나노기공물질의 특성은 기반물질의 특성과 더불어 기공의 형태, 크기, 분포에 의해서 결정된다. 나노기공물질의 기공에 대한 정보를 측정하는 방법으로는 TEM, 흡착법, FE-SEM과 더불어 중성자 또는 X-ray 빔의 산란을 이용하는 소각중성자산란 (Small-Angle Neutron Scatering, SANS), 소각 X-ray 산란 (Small-Angle X-ray Scattering, SAXS), 중성자반사율측정 (Neutron Relfectimetry, NR), X-ray 반사율측정 (X-Ray Reflectometry, XRR) 등이 사용되고 있다. 본 발표는 대략 1 nm - 100 nm 영역의 bulk 구조와 층상구조를 측정할 수 있는 소각 중성자 산란과 중성자 반사율 측정기법을 이용한 나노기공 측정기술을 다룬다.

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Characterization of Interface in Hybrid Composites (혼성복합재료의 계면 특성 분석)

  • Ha, Chang-Sik;Ahn, Ki Youl;Cho, Won-Jei
    • Journal of Adhesion and Interface
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    • v.1 no.1
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    • pp.47-55
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    • 2000
  • In this article, the characterization of the interface of hybrid composites was discussed. Interfacial interaction in organic/inorganic hybrid composites, especially silica-containing hybrids can be characterized by fluorescence spectroscopy, small angle X-ray scattering (SAXS), scanning electron microscopy (SEM), atomic force microscopy (AFM), and $^{29}Si$ NMR spectroscopy measurements.

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Mechanical and Thermal Properties of Epoxy/Organically Modified Mica Type Silicate (OMTS) Nanocomposites (에폭시/유기치환된 실리케이트 나노복합체의 기계적 및 열적 성질에 관한 연구)

  • 노진영;김진환
    • Polymer(Korea)
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    • v.25 no.5
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    • pp.691-698
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    • 2001
  • Nanocomposites based on epoxy acid nanoclay were prepared employing organically modified mica type silicate (OMTS), diglycidyl ether of bisphenol A (DGEBA) type epoxy. curing agent (dicyandiamide; DICY), and catalyst (benzyl dimethyl amine; BDMA). Both melt mixing and solution mixing were und for the sample preparation and structural developments with curing reaction were analyzed using X-ray diffractometer (XRD) and small angle X-ray scattering (SAXS). Because of the different curing rate between extra-gallery and intra-gallery reactions of epoxy mixtures, only intercalated structure was observed for the sample prepared by melt mixing while fully exfoliated structure was observed for the sample prepared by solution mixing. Mechanical properties of exfoliated epoxy nanocomposite were investigated using a dynamic mechanical analyzer (DMA). The dynamic storage modulus of the nanocomposite in both glass and rubbery plateau regions were increased with increasing OMTS contents, but glass transition temperatures ($T_g$) remained unchanged. Thermal properties of epoxy nanocomposite were investigated using thermogravimetric (TGA) and limit oxygen index (LOI) methods. Thermal decomposition onset points and LOI values were increased with increasing OMTS contents due to barrier effects of OMTS sheets.

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