Microfocus wide-angle X-ray scattering of polymers crystallized in a fast scanning chip calorimeter

M. Drongelen, van; A.M.J.T. Meijer-Vissers; D. Cavallo; G. Portale; G. Vanden Poel; R. Androsch

doi:10.1016/j.tca.2013.04.007

Microfocus wide-angle X-ray scattering of polymers crystallized in a fast scanning chip calorimeter

M. Drongelen, van, A.M.J.T. Meijer-Vissers, D. Cavallo, G. Portale, G. Vanden Poel, R. Androsch

Processing and Performance

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Abstract

Microfocus wide-angle X-ray scattering (WAXS) has been applied for analysis of the polymorphism of isotactic polypropylene and polyamide 6 prepared in a fast scanning chip calorimeter (FSC). Samples with a typical mass of few hundred nanograms, and lateral dimension and thickness of about 100 m and 20 m, respectively, were exposed to a defined thermal history in the FSC and subsequently analyzed regarding the X-ray structure at ambient temperature using an intense synchrotron microfocused X-ray beam. The relaxed melt of isotactic polypropylene was cooled at rates of 40 K s-1 and 200 K s-1 which allowed formation of -crystals or mesophase, respectively. Polyamide 6 was isothermally crystallized at 95 ¿C and 180 ¿C which led to formation of -mesophase and -crystals, respectively. This study demonstrated,for the first time, that FSC polymer crystallization experiments could be completed and expanded by subsequent in situ structure analysis by X-ray scattering.

Original language	English
Pages (from-to)	33-37
Journal	Thermochimica Acta
Volume	563
DOIs	https://doi.org/10.1016/j.tca.2013.04.007
Publication status	Published - 2013

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@article{c99521936a4d4a63bf48d44295b22090,

title = "Microfocus wide-angle X-ray scattering of polymers crystallized in a fast scanning chip calorimeter",

abstract = "Microfocus wide-angle X-ray scattering (WAXS) has been applied for analysis of the polymorphism of isotactic polypropylene and polyamide 6 prepared in a fast scanning chip calorimeter (FSC). Samples with a typical mass of few hundred nanograms, and lateral dimension and thickness of about 100 m and 20 m, respectively, were exposed to a defined thermal history in the FSC and subsequently analyzed regarding the X-ray structure at ambient temperature using an intense synchrotron microfocused X-ray beam. The relaxed melt of isotactic polypropylene was cooled at rates of 40 K s-1 and 200 K s-1 which allowed formation of -crystals or mesophase, respectively. Polyamide 6 was isothermally crystallized at 95 ¿C and 180 ¿C which led to formation of -mesophase and -crystals, respectively. This study demonstrated,for the first time, that FSC polymer crystallization experiments could be completed and expanded by subsequent in situ structure analysis by X-ray scattering.",

author = "{Drongelen, van}, M. and A.M.J.T. Meijer-Vissers and D. Cavallo and G. Portale and {Vanden Poel}, G. and R. Androsch",

year = "2013",

doi = "10.1016/j.tca.2013.04.007",

language = "English",

volume = "563",

pages = "33--37",

journal = "Thermochimica Acta",

issn = "0040-6031",

publisher = "Elsevier B.V.",

}

TY - JOUR

T1 - Microfocus wide-angle X-ray scattering of polymers crystallized in a fast scanning chip calorimeter

AU - Drongelen, van, M.

AU - Meijer-Vissers, A.M.J.T.

AU - Cavallo, D.

AU - Portale, G.

AU - Vanden Poel, G.

AU - Androsch, R.

PY - 2013

Y1 - 2013

N2 - Microfocus wide-angle X-ray scattering (WAXS) has been applied for analysis of the polymorphism of isotactic polypropylene and polyamide 6 prepared in a fast scanning chip calorimeter (FSC). Samples with a typical mass of few hundred nanograms, and lateral dimension and thickness of about 100 m and 20 m, respectively, were exposed to a defined thermal history in the FSC and subsequently analyzed regarding the X-ray structure at ambient temperature using an intense synchrotron microfocused X-ray beam. The relaxed melt of isotactic polypropylene was cooled at rates of 40 K s-1 and 200 K s-1 which allowed formation of -crystals or mesophase, respectively. Polyamide 6 was isothermally crystallized at 95 ¿C and 180 ¿C which led to formation of -mesophase and -crystals, respectively. This study demonstrated,for the first time, that FSC polymer crystallization experiments could be completed and expanded by subsequent in situ structure analysis by X-ray scattering.

AB - Microfocus wide-angle X-ray scattering (WAXS) has been applied for analysis of the polymorphism of isotactic polypropylene and polyamide 6 prepared in a fast scanning chip calorimeter (FSC). Samples with a typical mass of few hundred nanograms, and lateral dimension and thickness of about 100 m and 20 m, respectively, were exposed to a defined thermal history in the FSC and subsequently analyzed regarding the X-ray structure at ambient temperature using an intense synchrotron microfocused X-ray beam. The relaxed melt of isotactic polypropylene was cooled at rates of 40 K s-1 and 200 K s-1 which allowed formation of -crystals or mesophase, respectively. Polyamide 6 was isothermally crystallized at 95 ¿C and 180 ¿C which led to formation of -mesophase and -crystals, respectively. This study demonstrated,for the first time, that FSC polymer crystallization experiments could be completed and expanded by subsequent in situ structure analysis by X-ray scattering.

U2 - 10.1016/j.tca.2013.04.007

DO - 10.1016/j.tca.2013.04.007

M3 - Article

SN - 0040-6031

VL - 563

SP - 33

EP - 37

JO - Thermochimica Acta

JF - Thermochimica Acta

ER -

Microfocus wide-angle X-ray scattering of polymers crystallized in a fast scanning chip calorimeter

Abstract

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