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Related Experiment Videos

A TEM study on melt-crystallized poly(butylene terephthalate).

Norio Manabe1, Yoshimitsu Yokota, Hiroaki Minami

  • 1Suzuka Research Laboratory, Sumitomo Wiring Systems Co, Ltd, Mie, Japan.

Journal of Electron Microscopy
|May 11, 2002
PubMed
Summary

Ruthenium tetraoxide staining optimizes TEM observation of poly(butylene terephthalate) (PBT) crystals. This study reveals early fringed-micellar nuclei and later folded-chain crystals during melt crystallization.

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Area of Science:

  • Polymer Science
  • Materials Science
  • Crystallography

Background:

  • Poly(butylene terephthalate) (PBT) exhibits a low glass transition temperature (Tg ≈ 23°C), complicating its observation via Transmission Electron Microscopy (TEM).
  • Accurate morphological studies of PBT crystals are crucial for understanding its material properties and processing behavior.

Purpose of the Study:

  • To determine optimal ruthenium tetraoxide (RuO4) staining conditions for TEM observation of melt-grown PBT crystals.
  • To investigate the crystallization morphology of PBT at different stages and temperatures.

Main Methods:

  • Optimized ruthenium tetraoxide staining protocol for PBT samples.
  • Preparation of ultrathin sections of melt-grown PBT crystals.
  • Morphological analysis using Transmission Electron Microscopy (TEM).

Related Experiment Videos

  • Quantitative analysis of crystal thickness.

    • Main Results:

    • Optimal staining achieved at 25°C for 8 hours, enabling clear TEM visualization.
    • Early-stage isothermal crystallization (40°C) revealed fringed-micellar crystal nuclei.
    • Later stages showed the development of folded-chain fringed-micellar crystals.
    • Quantitative analysis indicated an increased fraction of chain-folded crystals with higher crystallization temperatures.

    Conclusions:

    • The developed RuO4 staining method is effective for TEM studies of low-Tg polymers like PBT.
    • PBT crystallization from the melt proceeds through fringed-micellar structures, evolving into folded-chain crystals.
    • Crystallization temperature significantly influences the final crystal morphology in PBT.