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

Search Result 47, Processing Time 0.021 seconds

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
    • /
    • v.10 no.1
    • /
    • pp.2-12
    • /
    • 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.

Olefin Separation Performances and Coordination Behaviors of Facilitated Transport Membranes Based on Poly(styrene-b-isoprene-b-styrene)/Silver Salt Complexes

  • Lee, Dong-Hoon;Kang, Yong-Soo;Kim, Jong-Hak
    • Macromolecular Research
    • /
    • v.17 no.2
    • /
    • pp.104-109
    • /
    • 2009
  • Solid-state facilitated, olefin transport membranes were prepared by complexation of poly(styrene-b-iso-prene-b-styrene) (SIS) block copolymer and silver salt. Facilitated olefin transport was not observed up to a silver mole fraction of 0.14, representing a threshold concentration, above which transport increased almost linearly with increasing silver salt concentration. This was because firstly the silver ions were selectively coordinated with the C=C bonds of PI blocks up to a silver mole fraction of 0.20, and secondly the coordinative interaction of the silver ions with the aliphatic C=C bond was stronger than that with the aromatic C=C bond, as confirmed by FT-Raman spectroscopy. Small angle X-ray scattering (SAXS) analysis showed that the cylindrical morphology of the neat SIS block copolymer was changed to a disordered structure at low silver concentrations ($0.01{\sim}0.02$). However, at intermediate silver concentrations ($0.15{\sim}0.20$), disordered-ordered structural changes occurred and finally returned to a disordered structure again at higher silver concentrations (>0.33). These results demonstrated that the facilitated olefin transport of SIS/silver salt complex membrancs was significantly affected by their coordinative interactions and nano-structural morphology.

Selective Coordination of Silver Ions to Poly(styrene-b-(ethylene-co-butylene)-b-styrene) and its Influence on Morphology and Facilitated Olefin Transport

  • Lee, Dong-Hoon;Kang, Yong-Soo;Kim, Jong-Hak;Kang, Sang-Wook
    • Macromolecular Research
    • /
    • v.16 no.8
    • /
    • pp.676-681
    • /
    • 2008
  • The $\pi$-complex membranes of poly(styrene-b-(ethylene-co-butylene)-b-styrene) (SEBS) of two silver salts of $AgBF_4$ and $AgCF_3SO_3$ were prepared and tested for the separation of the propylene/propane mixtures. The Fourier-transform infrared (FT-IR) spectra of these complexes showed that the silver salts were dissolved in SEBS up to a silver mole fraction of 0.14, due to $\pi$-complexation between the aromatic C=C bonds of styrene blocks and silver ions. Above this solubility limit, ion pairs and high-order ionic aggregates began to form, so that silver salts were distributed unselectively in both the EB and PS blocks. The domain size of the PS blocks was enlarged up to this critical concentration with increasing silver concentration without structural transitions, as confirmed by small angle x-ray scattering (SAXS). These structural properties of the SEBS/silver salt complexes may explain the lower separation properties for propylene/propane mixtures compared to poly(styrene-b-butadiene-b-styrene)(SBS)/silver salt complex membranes.

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

  • Kim, Eu-gene;Kim, Hwa-Joong
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
    • /
    • v.17 no.11
    • /
    • pp.1218-1223
    • /
    • 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.

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
    • /
    • v.10 no.6
    • /
    • pp.325-331
    • /
    • 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.

Small Angle X-ray Scattering Studies on Deformation Behavior of Rubber Toughened Polycarbonate (소각 X-선 산란을 이용한 고무입자로 강인화된 폴리카보네이트의 변형에 관한 연구)

  • Cho, Kilwon;Choi, Jaeseung;Yang, Jaeho;Kang, Byoung Il
    • Journal of Adhesion and Interface
    • /
    • v.3 no.4
    • /
    • pp.19-26
    • /
    • 2002
  • In order to study the toughening mechanism of rubber modified polycarbonate, the sequence of development of micro-voids was investigated by real-time small angle X-ray scattering with Synchrotron radiation (SR-SAXS). The used test method was wedge test. The scattering intensity increases with increasing penetration depth of wedge, i.e. applied strain. The increase is due to the micro-void formation during deformation. This micro-void was uniformly developed in matrix and was different from large-void due to internal cavitation of rubber particle and/or debonding between rubber particle and polycarbonate matrix. The micro-void was developed at the critical strain and the radius of micro-void is around $600{\AA}$. Above the critical strain the size of micro-void remains almost constant with increasing applied strain. However, the population of micro-void increased with applied strain.

  • PDF

Mechanism of Morphological Transition from Lamellar/Perforated Layer to Gyroid Phases

  • Ahn, Jong-Hyun;Zin, Wang-Cheol
    • Macromolecular Research
    • /
    • v.11 no.3
    • /
    • pp.152-156
    • /
    • 2003
  • We investigated epitaxial relations of phase transitions between the lamellar (L), hexagonally perforated layers (HPL), and gyroid (G) morphologies in styrene-isoprene diblock copolymer (PSI) and polyisoprene (PI)/PSI blend using rheology and small angle X-ray scattering (SAXS) techniques. In HPLlongrightarrowG transitions, six spot patterns of G phase were observed in two-dimensitional SAXS pattern. On the other hand, in direct L-longrightarrowG transition without appearance of HPL phase, the polydomain patterns of G phase were observed. From present study, it was understood that direct LlongrightarrowG transition of blend may be suppressed by high-energy barrier of transition and mismatches in domain orientation between epitaxially related lattice planes.

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

  • Ha, Chang-Sik;Ahn, Ki Youl;Cho, Won-Jei
    • Journal of Adhesion and Interface
    • /
    • v.1 no.1
    • /
    • pp.47-55
    • /
    • 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.

  • PDF