Thermal analysis, X-ray and electron diffraction studies on crystalline phase transitions in solvent-treated poly(hexamethylene terephthalate)

Ming Chien Wu, Eamor Woo, Taiyo Yoshioka, Masaki Tsuji

Research output: Contribution to journalArticle

12 Citations (Scopus)

Abstract

The crystal polymorphism, transformation, and morphologies in chloroform solvent-cast poly(hexamethylene terephthalate) (PHT) were examined by using differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD), and temperature in situ transmission electron microscopy (TEM). Solvent-induced crystallization of PHT at room temperature yielded an initial crystal of γ-form, as confirmed by WAXD. Upon DSC scanning, the original γ-form in PHT exhibited three endothermic peaks, whose origins and association were carefully analyzed. The first peak, much smaller than the other two, is in the temperature range of ca. 100-120 °C. It was found that the solvent-induced γ-form was transformed to β-form at 125 °C via a solid-to-solid transformation mechanism. In addition, WAXD showed that γ- and β-forms co-existed in the temperature range of 100-125 °C. These mixed crystal forms were further identified using TEM, and the selected-area electron diffraction (ED) patterns revealed that both γ- and β-form crystals co-existed and were packed within the same spherulite. Solid-solid transformation from the solvent-induced γ-form to β-form in PHT upon heat scanning was presented with evidence and discussed.

Original languageEnglish
Pages (from-to)5523-5530
Number of pages8
Journalpolymer
Volume47
Issue number15
DOIs
Publication statusPublished - 2006 Jul 12

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Electron diffraction
Thermoanalysis
Phase transitions
Crystalline materials
X ray diffraction
Crystals
Differential scanning calorimetry
Transmission electron microscopy
Scanning
Temperature
Chloroform
Chlorine compounds
Crystallization
Polymorphism
Diffraction patterns
Association reactions
terephthalic acid

All Science Journal Classification (ASJC) codes

  • Organic Chemistry
  • Polymers and Plastics
  • Materials Chemistry

Cite this

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title = "Thermal analysis, X-ray and electron diffraction studies on crystalline phase transitions in solvent-treated poly(hexamethylene terephthalate)",
abstract = "The crystal polymorphism, transformation, and morphologies in chloroform solvent-cast poly(hexamethylene terephthalate) (PHT) were examined by using differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD), and temperature in situ transmission electron microscopy (TEM). Solvent-induced crystallization of PHT at room temperature yielded an initial crystal of γ-form, as confirmed by WAXD. Upon DSC scanning, the original γ-form in PHT exhibited three endothermic peaks, whose origins and association were carefully analyzed. The first peak, much smaller than the other two, is in the temperature range of ca. 100-120 °C. It was found that the solvent-induced γ-form was transformed to β-form at 125 °C via a solid-to-solid transformation mechanism. In addition, WAXD showed that γ- and β-forms co-existed in the temperature range of 100-125 °C. These mixed crystal forms were further identified using TEM, and the selected-area electron diffraction (ED) patterns revealed that both γ- and β-form crystals co-existed and were packed within the same spherulite. Solid-solid transformation from the solvent-induced γ-form to β-form in PHT upon heat scanning was presented with evidence and discussed.",
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Thermal analysis, X-ray and electron diffraction studies on crystalline phase transitions in solvent-treated poly(hexamethylene terephthalate). / Wu, Ming Chien; Woo, Eamor; Yoshioka, Taiyo; Tsuji, Masaki.

In: polymer, Vol. 47, No. 15, 12.07.2006, p. 5523-5530.

Research output: Contribution to journalArticle

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AU - Wu, Ming Chien

AU - Woo, Eamor

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AU - Tsuji, Masaki

PY - 2006/7/12

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