Simultaneous measurements of small angle X‐ray scattering, wide angle X‐ray scattering and heat exchange during crystallization and melting of polymers

Bark, M.; Zachmann, H. G.

doi:10.1002/actp.1993.010440601

Cited by 36 publications

(22 citation statements)

References 25 publications

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“…The combination of x-ray based techniques like SAXS and WAXS is a logical step which has been implemented in several laboratories. [1][2][3] However, in recent years the tendency to combine SR x-ray scattering with further complementary techniques has gained widespread popularity. The possibility to not only obtain structural information but also elucidate the thermodynamic behavior, by means of thermal analysis, 4,5 has been shown to be particularly fruitful.…”

Section: Introductionmentioning

confidence: 99%

“…The possibility to not only obtain structural information but also elucidate the thermodynamic behavior, by means of thermal analysis, 4,5 has been shown to be particularly fruitful. Also the combination with light scattering, to elucidate large scale structures not accessible with x-rays in a timeresolved mode, 1 and Fourier transform infrared spectroscopy ͑FTIR͒ to monitor the chemical state of samples undergoing a chemical reaction, has been implemented. 6 Being able to implement the combination of SAXS, WAXS, and FTIR the logical next step in instrumentation is deemed to be the combination of x-ray scattering with Raman spectroscopy.…”

Section: Introductionmentioning

confidence: 99%

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Raman spectroscopy combined with small angle x-ray scattering and wide angle x-ray scattering as a tool for the study of phase transitions in polymers

Bryant

Gleeson

Ryan³

et al. 1998

Review of Scientific Instruments

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A novel combination of simultaneous experimental techniques has been developed as a tool for the study of phase transitions in polymers. Based upon a small angle x-ray scattering ͑SAXS͒ synchrotron radiation beamline it has been shown to be feasible to collect, in addition to the time-resolved SAXS data, wide angle x-ray scattering and Raman spectroscopy data with a time resolution of a few seconds.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Raman spectroscopy combined with small angle x-ray scattering and wide angle x-ray scattering as a tool for the study of phase transitions in polymers

Bryant

Gleeson

Ryan³

et al. 1998

Review of Scientific Instruments

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“…The simultaneous recording of time-resolved smallangle scattering (TRSAXS) and wide-angle scattering (TRWAXS) patterns has become increasingly popular in the last decade owing to the increasing number of SR beamlines suitable for this type of work (Bark & Zachmann, 1993;Bras et al, 1993;Hsiao, Gardner, Wu & Chu, 1993). The pioneering work on time-resolved scattering experiments on polymers by the group of Zachmann in Hamburg especially deserves to be mentioned (Zachmann & Gehrke, 1986).…”

Section: Introductionmentioning

confidence: 99%

Time-Resolved Small-Angle X-ray Scattering Combined with Wide-Angle X-ray Scattering

Bras¹,

Ryan²

1997

J Appl Cryst

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The high X-ray intensity of synchrotron radiation (SR) beamlines makes it possible to perform time-resolved small-angle X-ray scattering (SAXS) experiments. The information that can be obtained by collecting the wideangle diffraction pattern simultaneously not only increases the information content of an experiment but also increases the reliability of the time-correlations between SAXS and WAXS (wide-angle X-ray scattering) patterns. This is a great advantage for experiments with a time resolution below the level of 1 s per frame. With appropriate instrumentation, this is a time domain that is routinely accessible for a large group of research fields. This has had a considerable impact upon the understanding of fundamental aspects of phase transformations. Not only fundamental processes but also more applied fields have benefited from these developments. In polymer research this has led to a situation in which it has become possible to simulate materials processing techniques on-line. With the advent of thirdgeneration synchrotron-radiation sources (e.g. ESRF, APS, Spring8), it has become possible to develop SAXS/WAXS beamlines that will open up new research opportunities by utilizing the higher intensity, the tuneability and the higher collimation offered by these SR sources. However, some of the instrumentation limits in detector and sample environments that have become apparent in research on second-generation synchrotron-radiation sources still have not been appropriately addressed, which means that in some fields it will not be possible to take full advantage of the superior X-ray beam quality that third-generation synchrotrons can offer. A way in which these instrumentation limits can be overcome is discussed, and the instrumentation for a new bending-magnet beamline at the ESRF is used as an example.

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“…Advances have been made at DESY in Germany, Zachmann [23] made the first attempt at combining time-resolved WAXS and SAXS to study PET and its related liquid crystalline polymers. Due to the experimental arrangement used (vidicon and linear detectors) the data had a poor signal to noise ratio at DSC heating rates.…”

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confidence: 99%

“…Although their camera had good spatial resolution in both the small and wide angle regimes the angular range for WAXS was limited by the use of a linear detector to * 10° of arc and the SAXS camera was compromised by under focused Kratky optics At Daresbury we have recently constructed a SAXS/WAXS camera on a high intensity, highly-collimated beam line optimised for isotropic scatterers and equipped with a quadrant detector for SAXS and a curved detector for WAXS that covered > 70° of arc [28,29]. The problems associated with the two previously reported set-ups [23,25]were mainly alleviated. The experimental set-up has been described in detail [29] and its context reviewed [30].…”

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confidence: 99%

Polymer Structure Determination Using Simultaneous Small- and Wide-Angle X-ray Scattering and Differential Scanning Calorimetry

Ryan

Naylor

Komanschek

et al. 1994

ACS Symposium Series

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Experimental technique for the characterisation of the thermal--morphological properties of materials by X-ray scattering have been developed at Daresbury. Many thermal events, for example melting endotherms, are signals of phase transitions and thus changes in morphology. Collection of DSC and X-ray patterns simultaneously aids interpretation of the thermal behaviour. In many systems that morphology covers size-scales from the atomic to the microscopic, i.e. Å to μm. There are obvious advantages in collecting both the wide angle (sizes from 1 to 20 Å) and small angle (sizes from 20 to 1000 Å) X-ray patterns simultaneously to unambiguously characterise such thermal events. The new SAXS/WAXS technique makes this possible with a time resolution of 0.1 second which allows heating rates up to 120 °C min -1 . Simultaneous SAXS/DSC and SAXS/WAXS techniques are shown to provide an unambiguous method to follow the structural changes taking place during the programmed heating of a range of multiphase polymeric materials. The principles of the experiments are illustrated with specific examples of polyethylene terepthalate, high density polyethylene and block copolyurethanes.The experimental technique of DSC or DTA is often used in the thermal characterisation of structure-property-relations in polymers [1]. The phenomena investigated, such as melting and glass transitions in semi-crystalline polymers or the glass transitions of blends, are associated with strong morphological features. Much of the knowledge concerning the crystallisation of polymers comes from the application of programmed heating and cooling, and isothermal crystallisation studies by DSC combined with postmortem assessment of morphology by either X-ray diffraction or microscopy. Similarly, the existence of phase separation in polymer blends [2] or microphase separation in block copolymers [3] is often assessed by DSC with confirmation sought by scattering, microscopy and dynamic mechanical thermal analysis. The kinetics of

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Simultaneous measurements of small angle X‐ray scattering, wide angle X‐ray scattering and heat exchange during crystallization and melting of polymers

Cited by 36 publications

References 25 publications

Raman spectroscopy combined with small angle x-ray scattering and wide angle x-ray scattering as a tool for the study of phase transitions in polymers

Raman spectroscopy combined with small angle x-ray scattering and wide angle x-ray scattering as a tool for the study of phase transitions in polymers

Time-Resolved Small-Angle X-ray Scattering Combined with Wide-Angle X-ray Scattering

Polymer Structure Determination Using Simultaneous Small- and Wide-Angle X-ray Scattering and Differential Scanning Calorimetry

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