Polymer crystallization studies under processing-relevant conditions at the SAXS/WAXS DUBBLE beamline at the ESRF

Portale, Giuseppe; Cavallo, Dario; Alfonso, Giovanni Carlo; Hermida‐Merino, Daniel; Drongelen, Martin van; Balzano, Luigi; Peters, Gwm Gerrit; Goossens, Jgp Han; Bras, Wim

doi:10.1107/s0021889813027076

Cited by 117 publications

(105 citation statements)

References 61 publications

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“…Wide angle X-ray diffraction (WAXD) measurements during tensile deformation were performed at the beamline BM26B-DUBBLE of the ESRF, 23 focusing on the structural evolution of crystalline form II samples during the deformation. The sample clamps were properly aligned as such that the wider surface of the sample was oriented perpendicular to the X-ray beam.…”

Section: Methodsmentioning

confidence: 99%

Kinetics of the Polymorphic Transition in Isotactic Poly(1-butene) under Uniaxial Extension. New Insights From Designed Mechanical histories.

et al. 2014

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Isotactic poly(1-butene) (i-PBu) crystallizes upon cooling from the melt in a metastable tetragonal structure (form II), which slowly evolves toward the state of ultimate stability, i.e., the trigonal form I. It is well-known that this polymorphic transformation, which typically requires few weeks at room temperature, can be greatly accelerated by the application of mechanical stresses and/or deformation. However, the exact mechanism of this kinetics enhancement is not completely understood. In this work, the polymorphic transformation of i-PBu under tensile deformation is investigated in details. Thanks to properly designed mechanical histories−including experiments at different true strain and true stress rates−and to in situ wide-angle X-ray diffraction experiments, the role of the various deformation parameters is elucidated. The use of different time scales during the experiments enabled us to gain kinetics data on the transition, information which is disregarded in current literature. The set of experiments performed permit to highlight a stress-driven mechanism, active up to a fraction of transformed form I of about 0.4−0.5. After this value is reached, the stress-transformation time superposition principle does not hold anymore and the transition kinetics slows down, since a major part of the total applied stress is carried by the mechanically stronger form I lamellae.

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Section: Methodsmentioning

confidence: 99%

Kinetics of the Polymorphic Transition in Isotactic Poly(1-butene) under Uniaxial Extension. New Insights From Designed Mechanical histories.

et al. 2014

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“…In this paper, we first give a detailed description of the setup and how it has been successfully installed at the DUBBLE BM26B, 33 SixS, and SAMBA 34 beamlines at the European Synchrotron Radiation Facility (ESRF) and SOLEIL synchrotrons. To illustrate the functionality, examples will be discussed of in situ XRF and GISAXS measurements during ALD growth of ruthenium.…”

Section: Introductionmentioning

confidence: 99%

Mobile setup for synchrotron based in situ characterization during thermal and plasma-enhanced atomic layer deposition

Dendooven

Solano

Minjauw

et al. 2016

Review of Scientific Instruments

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We report the design of a mobile setup for synchrotron based in situ studies during atomic layer processing. The system was designed to facilitate in situ grazing incidence small angle x-ray scattering (GISAXS), x-ray fluorescence (XRF), and x-ray absorption spectroscopy measurements at synchrotron facilities. The setup consists of a compact high vacuum pump-type reactor for atomic layer deposition (ALD). The presence of a remote radio frequency plasma source enables in situ experiments during both thermal as well as plasma-enhanced ALD. The system has been successfully installed at different beam line end stations at the European Synchrotron Radiation Facility and SOLEIL synchrotrons. Examples are discussed of in situ GISAXS and XRF measurements during thermal and plasma-enhanced ALD growth of ruthenium from RuO4 (ToRuS™, Air Liquide) and H2 or H2 plasma, providing insights in the nucleation behavior of these processes.

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“…Hence, Θ ¼ 1 if shear has no effect and increases with shear rate. Ex-situ wide-angle X-ray diffraction (WAXD) single-shot experiments were performed on the solidified samples at the Dutch-Belgian (DUBBLE) beamline BM26 [88] of the European Synchroton Radiation Facility (Grenoble, France) using a high-resolution Pilatus 1M detector and a wavelength of λ ¼ 1.033 Å. Two-dimensional (2D) images were acquired and corrected for spatial distortion and for scattering of the empty sample cell [82]. Volume fractions of α-, β-, and γ-phases were obtained from WAXD images, as described by van Erp et al [82].…”

Section: Extended Dilatometrymentioning

confidence: 99%

Modeling Flow-Induced Crystallization

Roozemond

Drongelen

Peters

2016

Polymer Crystallization II

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A numerical model is presented that describes all aspects of flow-induced crystallization of isotactic polypropylene at high shear rates and elevated pressures. It incorporates nonlinear viscoelasticity, including viscosity change as a result of formation of oriented fibrillar crystals (shish), compressibility, and nonisothermal process conditions caused by shear heating and heat release as a result of crystallization. In the first part of this chapter, the model is validated with experimental data obtained in a channel flow geometry. Quantitative agreement between experimental results and the numerical model is observed in terms of pressure drop, apparent crystallinity, parent/daughter ratio, Hermans' orientation, and shear layer thickness. In the second part, the focus is on flow-induced crystallization of isotactic polypropylene at elevated pressures, resulting in multiple crystal phases and morphologies. All parameters but one are fixed a priori from the first part of the chapter. One additional parameter, determining the portion of β-crystal spherulites nucleated by flow, is introduced. By doing so, an accurate description of the fraction of β-phase crystals is obtained. The model accurately captures experimental data for fractions of all crystal phases over a wide range of flow conditions (shear rates from 0 to 200 s À1 , pressures from 100 to 1,200 bar, shear temperatures from 130 C to 180 C). Moreover, it is shown that, for high shear rates and pressures, the measured γ-phase fractions can only be matched if γ-crystals can nucleate directly on shish.

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Polymer crystallization studies under processing-relevant conditions at the SAXS/WAXS DUBBLE beamline at the ESRF

Cited by 117 publications

References 61 publications

Kinetics of the Polymorphic Transition in Isotactic Poly(1-butene) under Uniaxial Extension. New Insights From Designed Mechanical histories.

Kinetics of the Polymorphic Transition in Isotactic Poly(1-butene) under Uniaxial Extension. New Insights From Designed Mechanical histories.

Mobile setup for synchrotron based in situ characterization during thermal and plasma-enhanced atomic layer deposition

Modeling Flow-Induced Crystallization

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