CMOS flatpanel detectors for SAXS/WAXS experiments

Ogawa

Takano

et al. 2011

Self Cite

116

Scientific and engineering research on soft materials requires precise structural analysis to understand their hierarchical and fluctuating nature. A new beamline, the BL03XU frontier soft-material beamline, that is dedicated to scattering experiments on soft materials was recently installed at the third-generation synchrotron facility, SPring-8, in Japan. The BL03XU uses an in-vacuum undulator, and the photon flux of the obtained X-ray can reach 10 13 photons sec À1 , with an energy resolution of DE/EE2Â10 À4 at 12.4 keV. The BL03XU has two experimental hutches: a front one that is used for grazing-incidence scattering experiments and a second one for transmitting scattering experiments, which enables simultaneous small-and wide-angle X-ray scattering. The present paper introduces details about the instrument and some of the first scattering data measured at BL03XU, which reveals its cutting-edge design and high level of performance. INTRODUCTIONSoft materials represent a wide range of organic compounds that include polymers, colloids, surfactants and membranes. They exist in a variety of physical states that include semicrystallite, amorphous and glassy states, as well as liquid, thin film and micelle states. They are indispensably important materials in our daily lives as well as in modern industry. From a morphological point of view, they all share common features: fuzziness and hierarchy, which originate in the assembled structure of their constituent molecules and the timedependent fluctuations of their structure. Understanding the physical properties of soft materials and thus controlling and providing functionality requires accurate characterization of their fuzziness and hierarchy. Their constituent molecules are organized into mesoscopic structures that are larger than atoms and molecules, but much smaller than the macroscopic scale of the materials. The required observation scale can therefore range from B10 À1 to 10 4 nm. The X-ray scattering technique, which has a combination of wide-and small-angle measurements, is one of the best tools to use in characterizing such systems. In addition, the fragile and hierarchical objects generally

Section: Multipurpose Soft-materials Beamline H Masunaga Et Almentioning

confidence: 99%

Multipurpose soft-material SAXS/WAXS/GISAXS beamline at SPring-8

Ogawa

Takano

et al. 2011

Self Cite

116

“…To reduce the scattering from the air, vacuum paths of 0.5 m (VP1) and 1.0 m (VP2) in length can be used for the measurements that use a camera length of 1.0 and 2.0 m, respectively. For the simultaneous measurements of the GIWAXS and the GISAXS, a flat panel detector (Hamamatsu Photonics; C9827DK-10) 13 was utilized behind the sample position to cover a quadrant in the q range of 5-30 nm À1 for the GIWAXS measurements. Table 1 summarizes the specifications of each measurement at the wavelength l of 1.0 Å for typical experiments.…”

Section: Experimental Procedures Instrument Componentsmentioning

confidence: 99%

Experimental station for multiscale surface structural analyses of soft-material films at SPring-8 via a GISWAX/GIXD/XR-integrated system

Ogawa

Sasaki

et al. 2012

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To gain a better understanding of the function of soft-material thin films, one should investigate the multiscale structural information from the surface roughness down to the atomically truncated structures at microarea. To achieve such an integrated investigation, a new experimental system has been launched by coupling with the measurement techniques, which include grazing incidence small/wide-angle X-ray scattering (GISWAXS) and grazing incidence X-ray diffraction (GIXD), as well as X-ray reflectivity (XR), at the BL03XU beamline of SPring-8. The high brilliance and low divergence beam allows the surface and interface structure measurements from the angstrom to the micrometer scale using a soller-slit system for proper optimization of measurement precision. A typical structural analysis of the soft-material film was performed to evaluate the practical performance and specifications of the experimental system.

“…The combination of the ultra-bright X-ray beams with highlysensitive detectors makes it possible to perform the above-mentioned in situ WAXD/SAXS simultaneous measurements satisfactorily. [3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20][21] In the European Synchrotron Radiation Facility (ESRF), 6 The Advance Photon Source (APS), 7,8 and the other synchrotron radiation facilities, for example, the WAXD/SAXS simultaneous measurement system with two-dimensional (2D) detectors (2D-WAXD/SAXS measurement system) is a default utilized for many general users, helping them to create many papers on the structural evolution process of polymers. In SPring-8 and Photon Factory, the WAXD/SAXS simultaneous measurements were carried our by the limited numbers of technically-skilled particular researchers.…”

mentioning

confidence: 99%

“…In SPring-8 and Photon Factory, the WAXD/SAXS simultaneous measurements were carried our by the limited numbers of technically-skilled particular researchers. [13][14][15][16][17]20,21 As mentioned above, the 2D-WAXD/ SAXS measurement system is a necessary tool for kinetic investigations on the hierarchical structure of polymers.…”

mentioning

confidence: 99%

“…Yagi and Inoue performed the WAXD/SAXS measurements to test the ability of a new type detector called a CMOS FPD at the BL40XU and the BL40B2 in SPring-8. 21 Also, Amemiya et al reported the experimental results obtained using a FP detector. 15 Ito et al reported the WAXD/SAXS data of biodegradable polymers measured with the taper optics fiber CCD detector as a detector for WAXD.…”

mentioning

confidence: 99%

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Development of Synchrotron DSC/WAXD/SAXS Simultaneous Measurement System for Polymeric Materials at the BL40B2 in SPring-8 and its Application to the Study of Crystal Phase Transitions of Fluorine Polymers

Sasaki

Tashiro

et al. 2007

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ABSTRACT:A new system of rapidly-scanning DSC/WAXD/SAXS simultaneous measurements has been successfully developed at the BL40B2 in SPring-8, Japan. The combination of the ultra-bright and highly-directional X-ray beams with the highly-sensitive two-dimensional (2D) detectors such as an imaging plate (IP), a CCD detector and a flat panel (FP) detector has made it possible to perform the rapidly-scanning time-resolved measurements of WAXD and SAXS for the polymeric materials subjected to the various kinds of external field like temperature, tensile force, magnetic field, hydrostatic pressure, and so on. The experimental data about the phase transitions of vinylidene fluoridetrifluoroethylene copolymer with VDF 82 mol % content and poly(vinylidene fluoride) form I have been presented as actual examples, where the phase transitions of the polar crystal consisting of planar-zigzag chains to the gauche-type high-temperature phase have been confirmed definitely and the remarkable change in lamellar stacking structure could be detected in the temperature region immediately below the melting point. [doi:10.1295/polymj.PJ2007105] KEY WORDS Simultaneous Measurement System / Wide-angle X-ray Diffraction / Small-angle X-ray Scattering / Differential Scanning Calorimetry / SPring-8 / Poly(vinylidene fluoride) / Phase Transition / Polymeric materials consist of complicated aggregation state of chains. In the case of semicrystalline polymer, for example, these chains gather together to form the crystalline region or a crystalline lamella. These lamellae are stacked together to construct a spherulite. There are amorphous region between these stacked lamellae. In the spherulite, the lamellae extend and twist periodically from the spherulitic center along the radial direction, giving the so-called extinction ring in its polarized optical microscopic image. It is essentially important to clarify the evolution process of this complicated hierarchical structure of polymers from the various viewpoints on angstrom-tomicrometer scale in order to design and control their physical and structural properties. One of the most useful and quantitative methods for attainment of this purpose is to use the X-ray scattering technique. The wide-angle X-ray diffraction (WAXD) gives us information on the chain conformation and the aggregation state of chains in the crystalline and amorphous regions. The small-angle X-ray scattering (SAXS) tells us about the rough form of molecular chains, the aggregation structure of crystalline lamellae, and so on. Therefore, the time-resolved measurements of WAXD and SAXS allow us to trace the structural evolution process of polymers in the heating or cooling process, for example. There were many reports on the WAXD and/or SAXS experimental data.1 In most cases the WAXD or SAXS measurement was performed for a sample separately by assuming the reproducibility of the experimental conditions. But, strictly speaking, we do not have any guarantee about the reproducibility of the experimental conditions in the WAXD and S...