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Poly(ethylene oxide) Crystallization within a One-Dimensional Defect-Free Confinement on the Nanoscale

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Maurice Morton Institute and Department of Polymer Science, The University of Akron, Akron, Ohio 44325-3909; Institut de Chimie des Surfaces et Interfaces, UPR CNRS 9069, 15 rue Jean Starcky, B.P. 2488, 68057 Mulhouse Cedex, France; Department of Materials Science and Engineering, Massachusetts Institute and Technology, Cambridge, Massachusetts 02139; and Institut Charles Sadron, 23, Rue du Loess, Strasbourg 67034, France
* To whom correspondence should be addressed. E-mail: [email protected]; [email protected]
†The University of Akron.
‡UPR CNRS 9069.
§Massachusetts Institute and Technology.
∥Institut Charles Sadron.
Cite this: Macromolecules 2008, 41, 13, 4794–4801
Publication Date (Web):June 6, 2008
https://doi.org/10.1021/ma8006619
Copyright © 2008 American Chemical Society
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    Abstract

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    A new approach was designed to study polymer crystallization in a one-dimensional (1D), defect-free, nanoscale confinement utilizing single crystals of poly(ethylene oxide)-block-polystyrene (PEO-b-PS) diblock copolymers as templates. The single crystals grown in dilute solution consisted of a PEO single crystal layer sandwiched between two PS layers formed by the tethered PS blocks on the PEO single crystal top and bottom basal surfaces. Transition behaviors of PEO-b-PS single crystals were investigated using differential scanning calorimetry, transmission electron microscopy, and atomic force microscopy. It was observed that the glass transition temperature of PS blocks in a thin film with a thickness of 7.2 nm is 71 °C, which is higher than the melting temperature of a PEO single crystal with a thickness of 7.9 nm (57 °C). Therefore, the PEO single crystal could be melted, and the PEO blocks could recrystallize in between these two vitrified PS layers when the temperature is brought down to generate sufficient supercooling. This recrystallization process of the PEO blocks was thus carried out in a 1D lamellar confinement without any defects. After the recrystallization, the crystal orientation change of the PEO crystals at different recrystallization temperatures (Trx) was monitored using electron diffraction (ED). First, it was found that the PEO blocks could not recrystallize at Trx > −5 °C, indicating absence of heterogeneous nucleation in the PEO blocks. This Trx of −5 °C corresponds to the starting temperature for homogeneous nucleation of PEO as reported previously. Second, crystallographic analyses of the ED obtained from the recrystallized PEO blocks show that for Trx < −20 °C the c-axis, and thus the PEO small crystals, possess a random orientation. When −20 °C ≤ Trx < −5 °C, the c-axis of the PEO crystals is parallel to the glassy PS basal plane and aligned with the a*- or b-axis of the original PEO-b-PS single crystal grown in dilute solution. The self-seeding technique was used for Trx > −5 °C to create heterogeneous nucleation. Here, the c-axis of PEO crystals was inclined with respect to the vitrified PS lamellar normal at an angle of about 26°.

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