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Synthesis of Narrow Molecular Weight Distribution Norbornene-Lactone Functionalized Polymers by Nitroxide-Mediated Polymerization: Candidates for 193-nm Photoresist Materials
Polymers 2014, 6(2), 583-600; doi:10.3390/polym6020583

Molecular Weight and Crystallization Temperature Effects on Poly(ethylene terephthalate) (PET) Homopolymers, an Isothermal Crystallization Analysis

1,* , 2
1 Centro de Ingeniería y Desarrollo Industrial, Av. Pie de la Cuesta No. 702, Desarrollo San Pablo, Querétaro, Qro. 76130, Mexico 2 Centro de Investigación en Química Aplicada, Blvd. Enrique Reyna Hermosillo 140, Col. San José de los Cerritos, Saltillo, Coah. 25294, Mexico 3 Universidad Autónoma de San Luis Potosí, Alvaro Obregon 64, San Luis Potosí, S.L.P. 78000, Mexico 4 Department of Chemistry, Stony Brook University, Stony Brook, NY 11794, USA
* Author to whom correspondence should be addressed.
Received: 19 December 2013 / Revised: 7 February 2014 / Accepted: 14 February 2014 / Published: 21 February 2014
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The isothermal crystallization of poly(ethylene terephthalate) (PET) homopolymers with different molecular weight was studied in a wide temperature range (140–230 °C) using different experimental techniques. Three different morphological regions, labeled r1, r2 and r3, were distinguished as a function of crystallization temperature (Tc). In r1 (low Tc) crystallized samples were characterized by a low crystalline degree with a small spherulite texture containing thin crystals. In r2 (intermediate Tc) samples showed medium size spherulites composed of two distinct crystalline families (thin and thick crystals). In this temperature range, the crystallization exhibited a maximum value and it was associated with a high content of secondary crystals. In r3 (high Tc), samples presented considerable amorphous zones and regions consisting of oversized spherulites containing only thick crystals. Time-resolved wide-angle X-ray diffraction measurements, using synchrotron radiation, indicated a rapid evolution of the crystalline degree within the second region, in contrast with the quite slow evolution observed in the third region. On the other hand, by small-angle X-ray scattering (SAXS) and time-resolved SAXS experiment, it was found that the long period (L) as well as the lamellar thickness (lc) increase as a function of Tc, corroborating the formation of the thickest crystals in the third region. From all these observations, a morphological model was proposed for each region.
Keywords: isothermal crystallization; PET; secondary crystallization; synchrotron radiation isothermal crystallization; PET; secondary crystallization; synchrotron radiation
This is an open access article distributed under the Creative Commons Attribution License (CC BY 3.0).

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Baldenegro-Perez, L.A.; Navarro-Rodriguez, D.; Medellin-Rodriguez, F.J.; Hsiao, B.; Avila-Orta, C.A.; Sics, I. Molecular Weight and Crystallization Temperature Effects on Poly(ethylene terephthalate) (PET) Homopolymers, an Isothermal Crystallization Analysis. Polymers 2014, 6, 583-600.

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