Specimen preparation method ultrathin sectioning

There are multiphase polymers where OM and SEM techniques cannot fully describe the microstructure due to a combination of small particle size (less than 0.5 /xm) and good adhesion between the dispersed phase and the matrix. Additionally, broad particle size distributions are often encountered, and in these cases a combination of techniques is required to describe the microstructure. TEM requires ultrathin specimens, about 50-500 nm or less in thickness, which are prepared by film casting or ultrathin sectioning. Films formed by casting or dipping methods provide a much easier specimen preparation method than ultrathin sectioning of bulk plastics. However, a major question in such studies is always whether the microstructure is the same as in bulk polymers of industrial interest. Specific stains are often required to provide contrast between the dispersed phase and the matrix pol)m[ier. 

Microscopy techniques can be used to evaluate the size and distribution of particles added to polymer fibers, such as metals that modify the physical, mechanical, or electrical properties. In general, ultrathin sections are examined in either STEM or TEM modes to reveal the particles within the polymer. Energy (EDS) and wavelength dispersive x-ray spectroscopy (WDS) methods are used to map for various elements in order to establish the relation between the particle morphology and chemical composition. A specimen preparation method for x-ray analysis in the SEM is to use a trimmed block face, which remains after cutting thin sections, or to study a thick section. An example of such a study is described below. 

Cellulose nitrate and cellulose acetate (CA) were among the first asymmetric, reverse osmosis membranes to be produced [121]. Plummer et al. [122] described 13 specimen preparation methods for observation of CA membrane structures. They pointed out the lack of contrast in epoxy embedded sections and that one of the best stains, osmium tetroxide, reacts with the polymer. Freeze fractured membranes were found by these authors to be of questionable value. In our experience, if care is taken, SEM study of fractured membranes can provide an informative view of the structure even though some structures collapse, and their sizes cannot be accurately determined. A method found acceptable was ultrathin sectioning of gelatin embedded wet membranes (TEM). The structure of CA membranes was shown by replication [123] and SEM [124]. 

In literature the following methods of preparation of polymer material specimen and studying their morphology are described methods of ultrathin section and films with contrasting of osmium tetroxide (10.11). method of replication of the brittle fractur-ed surface (11.12) oxygen and chemical etch of the polished surface or the fractured surface with the following replication for electron microscopy (11. 

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