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

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Structure Analysis of Liquid Crystal Emulsions Using X-ray Scattering Analysis (X선 산란분석법을 이용한 액정에멀젼 구조분석)

  • Park, So Hyun;Kim, Su Ji;Noh, Min Joo;Lee, Jun Bae;Park, Soo Nam
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.42 no.3
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    • pp.297-302
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    • 2016
  • In this study, we prepared liquid crystal emulsions composed of $C_{12-20}$ alkyl glucoside, $C_{14-22}$ alcohol, and behenyl alcohol and performed structure analysis using various analytical equipment. First, as an important characteristic of liquid crystal emulsions, maltese cross patterns and multi-layer structure were observed by a polarized microscope and cryo-SEM. Also, formation of liquid crystal phase was confirmed by DSC and multi-layer lamellar structure having an interlayer spacing approximately $305{\AA}$ was confirmed by small angle x-ray scattering (SAXS). The alkyl chain arrangement formed orthorhombic structure of a lamellar structure of the liquid crystal emulsion was confirmed by wide angle x-ray scattering (WAXS). These results suggest that information on the various physical properties obtained through the research of liquid crystal emulsion structure is expected to be widely used in cosmetics development in the future.

Competition between Phase Separation and Crystallization in a PCL/PEG Polymer Blend Captured by Synchronized SAXS, WAXS, and DSC

  • Chuang Wei-Tsung;Jeng U-Ser;Sheu Hwo-Shuenn;Hong Po-Da
    • Macromolecular Research
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    • v.14 no.1
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    • pp.45-51
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    • 2006
  • We conducted simultaneous, small-angle, X-ray scattering/differential scanning calorimetry (SAXS/DSC) and simultaneous, wide-angle, X-ray scattering (WAXS)/DSC measurements for a polymer blend of poly($\varepsilon$-caprolactone)/poly(ethylene glycol)(PCL/PEG). The time-dependent SAXS/DSC and WAXS/DSC results, measured while the system was quenched below the melting temperature of PCL from a melting state, revealed the competitive behavior between liquid-liquid phase separation and crystallization in the polymer blend. The time-dependent structural evolution extracted from the SAXS/WAXS/DSC results can be characterized by the following four stages in the PCL crystallization process: the induction (I), nucleation (II), growth (III), and late (IV) stages. The influence of the liquid-liquid phase separation on the crystallization of PCL was also observed by phase-contrast microscope and polarized microscope with 1/4$\lambda$ compensator.

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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Sol-Gel Transition in Di-(2-ethylhexyl) phthalate-Plasticized Poly(vinyl chloride)

  • Lee, Chang-Hyung;Nah, Jae-Woon;Cho, Kil-Won;Kim, Seong-Hun;Hahn, Ai-Ran
    • Bulletin of the Korean Chemical Society
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    • v.24 no.10
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    • pp.1485-1489
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    • 2003
  • The gelation for di-(2-ethylhexyl) phthalate (DEHP)-plasticized poly(vinyl chloride) was studied by measuring time-resolved small-angle X-ray scattering (SAXS) and a flow of the solutions in test tube. It was found that for the gelation there were three regimes. At Regime I, the solution rapidly changed to a gel, and the SAXS intensity showed a peak and the peak intensity increased, keeping the peak angle constant. Applying the SAXS intensity to the kinetic analysis of the liquid-liquid phase separation, it was revealed that the spinodal decomposition proceeded to develop a periodic length of 29.9 nanometer in size, a hydrogen-bonding-type association in polymer rich phase followed, and then it induced fast gelation rate. At Regime II, the gelation slowly occurred and the SAXS intensity was not observed, suggesting that a homogeneous gel network was formed by a hydrogen-bonding. At regime III, the solution was a homogeneous sol.

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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    • v.23 no.4
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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.

The Morphology, Structure and Melting Behaviour of Cold Crystallized Isotactic Polystyrene

  • Marega, Carla;Causin, Valerio;Marigo, Antonio
    • Macromolecular Research
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    • v.14 no.6
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    • pp.588-595
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    • 2006
  • The morphology, structure and melting behaviour of cold-crystallized isotactic polystyrene (iPS) were studied by differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD) and small angle X-ray scattering (SAXS). The polymer was found to crystallize according to the dual-lamellar stack model. The two populations of lamellae, along with a melting-recrystallization phenomenon, determined the appearance of multiple melting peaks in DSC traces. The annealing peak was attributed to the relaxation of a rigid amorphous phase, rather than to the melting of crystalline material.

Effect of Al Precursor Type on Mesoporous Alumina Particles Prepared by Spray Pyrolysis (분무열분해공정에 의한 메조기공 알루미나 제조에 있어 Al 전구체 영향)

  • Kim, Joo-Hyun;Jung, Kyeong-Youl;Park, Kyun-Young
    • Journal of Powder Materials
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    • v.17 no.3
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    • pp.209-215
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    • 2010
  • Mesoporous alumina particles were prepared by spray pyrolysis using cetyltrimethyl-ammonium bromide (CTAB) as a structure directing agent and the effect of Al precursor types on the texture properties was studied using $N_2$ adsorption isotherms, small-angle X-ray scattering (SAXS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The surface area and the microstructure of alumina particles were significantly influenced by the Al precursor type. The largest BET surface area was obtained when Al chloride was used, whereas alumina particles prepared from Al acetate had the largest pore volume. According to small-angle X-ray scattering (SAXS) analysis, the alumina powders prepared using nitrate and acetate precursors had a clear single SAXS peak around $2{\theta}=1.0{\sim}1.5^{\circ}$, indicating that regular mesopores with sponge-like structure were produced. On the basis of TEM, SAXS, and $N_2$ isotherm results, the chloride precursor was most profitable to obtain the largest surface area ($265\;m^2/g$), whereas, the nitrate precursor is useful for the preparation of non-hollow mesoporous alumina with regular pore size, maintaining high surface area (${\sim}233\;m^2/g$).

Sulfonated Polystyrene Ionomers Containing 4-Aminobenzoic Acid Studied by a Small-Angle X-Ray Scattering Technique

  • Song, Ju-Myung;Hong, Min-Chul;Kim, Joon-Seop;Jikang Yoo;Yu, Jeong-A;Kim, Whangi
    • Macromolecular Research
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    • v.10 no.6
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    • pp.304-310
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    • 2002
  • In a recent study by the same authors using a DMTA (Dynamic Mechanical Thermal Analyzer), it was found that the 4-aminobenzoic arid (ABA) molecules acted as either a neutralizing agent, or a plasticizer, or a filler, depending on the order of mixing of poly(styrene-co-styrenesulfonic acid) (PSSA), ABA, and NaOH. Subsequent to that study, we here pursued the same topic, i.e., the effect of the addition of CsOH (instead of NaOH) and ABA on the morphology of PSSA, but this time, by using a small-angle X-ray scattering (SAXS) technique. In line with the previous results, the present study with the SAXS technique verified that the order of mixing has a significant effect on the morphology of ionomers. In addition, with the SAXS data and the density values of the ionomers, we attempted to calculate both the number of sulfonate ionic groups per multiplet and the size of the multiplet of the ionomer.

A Study on the Liquid Crystal Formed in PLO Gel Containing Ceramide NP (Ceramide NP 를 함유한 PLO Gel 에서 형성되는 액정에 관한 연구)

  • Heo, Min Geun;Yoon, Kyung-Sup
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.47 no.1
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    • pp.85-92
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    • 2021
  • The stratum corneum is formed from keratinocytes and intercellular lipids, with ceramide as the main component of intercellular lipids. Ceramides are one of the important components of the intercellular lipids to form a lamellar structure, but they are insoluble and therefore are not suitable for direct application to the skin. Thus, it was intended to apply ceramide to the formulation of pluronic lecithin organogel (PLO gel), which received constant attention among drug delivery systems. A suitable oil for formulation was selected and a PLO gel containing ceramide was manufactured. Liquid crystal formation and variation were observed using polarized microscopes, and viscoelastic analysis was performed to find out the viscoelastic behavior of the PLO gel. Small-angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) analysis were performed to confirm the structures in the formulation. Results showed that the size and stability of the liquid crystal differed depending on the content ratio of ceramide and lecithin in the PLO gel containing ceramide. Furthermore, viscoelastic analysis showed the stability of the formulation, and SAXS/WAXS analysis confirmed that the PLO gel without ceramide had hexagonal structure of the quadrilateral system array, and the PLO gel with ceramide had the lamellar structure of the quadrilateral system array.

Small-Angle X-ray Scattering Station 4C2 BL of Pohang Accelerator Laboratory for Advance in Korean Polymer Science

  • Yoon, Jin-Hwan;Kim, Kwang-Woo;Kim, Je-Han;Heo, Kyu-Young;Jin, Kyeong-Sik;Jin, Sang-Woo;Shin, Tae-Joo;Lee, Byeong-Du;Rho, Ye-Cheol;Ahn, Byung-Cheol;Ree, Moon-Hor
    • Macromolecular Research
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    • v.16 no.7
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    • pp.575-585
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    • 2008
  • There are two beamlines (BLs), 4C1 and 4C2, at the Pohang Accelerator Laboratory that are dedicated to small angle X-ray scattering (SAXS). The 4C1 BL was constructed in early 2000 and is open to public users, including both domestic and foreign researchers. In 2003, construction of the second SAXS BL, 4C2, was complete and commissioning and user support were started. The 4C2 BL uses the same bending magnet as its light source as the 4C1 BL. The 4C1 BL uses a synthetic double multilayer monochromator, whereas the 4C2 BL uses a Si(111) double crystal monochromator for both small angle and wide angle X-ray scattering. In the 4C2 BL, the collimating mirror is positioned behind the monochromator in order to enhance the beam flux and energy resolution. A toroidal focusing mirror is positioned in front of the monochromator to increase the beam flux and eliminate higher harmonics. The 4C2 BL also contains a digital cooled charge coupled detector, which has a wide dynamic range and good sensitivity to weak scattering, thereby making it suitable for a range of SAXS and wide angle X-ray scattering experiments. The general performance of the 4C2 BL was initially tested using standard samples and further confirmed by the experience of users during three years of operation. In addition, several grazing incidence X-ray scattering measurements were carried out at the 4C2 BL.