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Related Experiment Videos

New controlled environment vitrification system for preparing wet samples for cryo-SEM.

H Ge1, W J Suszynski, H T Davis

  • 1Department of Chemical Engineering & Materials Science, University of Minnesota, Minneapolis, MN, USA.

Journal of Microscopy
|January 5, 2008
PubMed
Summary
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A new controlled environment vitrification system (CEVS) enables detailed cryogenic scanning electron microscopy (Cryo-SEM) of solvent-containing coatings. This system optimizes sample preparation for artifact-free microstructural analysis.

Area of Science:

  • Materials Science
  • Microscopy Techniques
  • Polymer Science

Background:

  • Analyzing solvent-containing coatings requires specialized techniques to preserve their microstructure.
  • Existing methods often introduce artifacts during sample preparation for microscopy.
  • Cryogenic scanning electron microscopy (Cryo-SEM) offers high-resolution imaging but demands rapid, artifact-free vitrification.

Purpose of the Study:

  • To design and construct a novel controlled environment vitrification system (CEVS).
  • To enable in-situ examination of coating microstructures in their initial suspension state using Cryo-SEM.
  • To minimize shear and freezing artifacts during the vitrification of solvent-containing samples.

Main Methods:

  • Development of a CEVS with main and subsidiary chambers for controlled drying and annealing.

Related Experiment Videos

  • Blade-coating of samples on silicon wafers within the CEVS.
  • Controlled plunging of samples into liquid ethane at their freezing point using an adjustable sample holder.
  • High-speed digital camera recording of the plunge process.
  • Interpretation of data using a new hypothesis on rapid cooling during vitrification.

    • Main Results:

    • The CEVS successfully facilitated the vitrification of latex, latex-composite, and other coatings.
    • Cryo-SEM examination revealed microstructural development in the presence of solvent.
    • Optimization of sample attitude during plunging was found crucial for balancing freezing rate and surface shearing.
    • The study provided insights into the cooling dynamics during vitrification.

    Conclusions:

    • The developed CEVS is effective for preparing solvent-containing coating samples for Cryo-SEM.
    • The system allows for artifact-free analysis of microstructural development.
    • Understanding and controlling the vitrification process, particularly sample attitude, is key to obtaining high-quality Cryo-SEM data.