title: Simultaneous Synchrotron WAXD and Fast Scanning (Chip) Calorimetry: On the (Isothermal) Crystallization of HDPE and PA11 at High Supercoolings and Cooling Rates up to 200 °C s(-1).
abstract: An experimental setup, making use of a Flash DSC 1 prototype, is presented in which materials can be studied simultaneously by fast scanning calorimetry (FSC) and synchrotron wide angle X-ray diffraction (WAXD). Accumulation of multiple, identical measurements results in high quality, millisecond WAXD patterns. Patterns at every degree during the crystallization and melting of high density polyethylene at FSC typical scanning rates from 20 up to 200 °C s(-1) are discussed in terms of the temperature and scanning rate dependent material crystallinities and crystal densities. Interestingly, the combined approach reveals FSC thermal lag issues, for which can be corrected. For polyamide 11, isothermal solidification at high supercooling yields a mesomorphic phase in less than a second, whereas at very low supercooling crystals are obtained. At intermediate supercooling, mixtures of mesomorphic and crystalline material are generated at a ratio proportional to the supercooling. This ratio is constant over the isothermal solidification time.
authors.affiliation: Polymer Chemistry and Materials, KU Leuven, Celestijnenlaan 200F - box 2404, B-3001, Leuven, Belgium.
authors.forename: Dorien
authors.initials: D
authors.lastname: Baeten
authors.affiliation: Polymer Chemistry and Materials, KU Leuven, Celestijnenlaan 200F - box 2404, B-3001, Leuven, Belgium.
authors.forename: Vincent B F
authors.initials: VB
authors.lastname: Mathot
authors.affiliation: Polymer Chemistry and Materials, KU Leuven, Celestijnenlaan 200F - box 2404, B-3001, Leuven, Belgium.
authors.forename: Thijs F J
authors.initials: TF
authors.lastname: Pijpers
authors.affiliation: Polymer Chemistry and Materials, KU Leuven, Celestijnenlaan 200F - box 2404, B-3001, Leuven, Belgium.
authors.forename: Olivier
authors.initials: O
authors.lastname: Verkinderen
authors.affiliation: DUBBLE CRG BM26@ESRF, Netherlands Organization for Scientific Research, 71 Avenue des Martyrs, Grenoble, 38043, France.
authors.forename: Giuseppe
authors.initials: G
authors.lastname: Portale
authors.affiliation: Soft Matter, Rheology and Technology, KU Leuven, Willem de Croylaan 46, B-3001, Leuven, Belgium.
authors.forename: Peter
authors.initials: P
authors.lastname: Van Puyvelde
authors.affiliation: Polymer Chemistry and Materials, KU Leuven, Celestijnenlaan 200F - box 2404, B-3001, Leuven, Belgium.
authors.forename: Bart
authors.initials: B
authors.lastname: Goderis
mesh_terms: D002152:Calorimetry, Differential Scanning; D003460:Crystallization; D020959:Polyethylene / Q000737:chemistry*; D011137:Polystyrenes / Q000737:chemistry*; D014961:X-Ray Diffraction
chemical_list: D011137:Polystyrenes; D020959:Polyethylene
keywords: crystallization; fast scanning (chip) calorimetry; morphology; polymers; synchrotron wide angle X-ray diffraction