Investigation of CPE/PVC morphology via STEM

Author(s):  
E. G. Rightor ◽  
E. I. Garcia-Meitin ◽  
D. W. Liou

Microscopic characterization of the phase morphology of poly(vinyl chloride) (PVC) modified with chlorinated polyethylene (CPE) is vital to understanding the blend physical properties. A 2-3 week CPE selective staining technique, developed by Fleischner et al., has been the mainstay for recent TEM investigations of CPE/PVC. Several researchers employing this method have reported a network structure of CPE surrounding primary PVC particles.Rapid electron beam-induced dehydrochlorination of chlorinated polymers prohibits TEM examination of unstained sections. Chemical changes resulting from such dehydrochlorination of polymers was addressed recently by Vesely and Finch. In this study we investigated unstained thin sections, obtained at ambient temperature with a diamond knife, by scanning transmission electron microscopy (STEM) on a JEOL 2000 FX.As the STEM micrographs show (Figs. 1-3), sufficient contrast was available to distinguish CPE (light phase) from the PVC matrix (dark). Differences in initial chlorine concentration and rates of beam-induced mass loss most likely account for the contrast between phases.

Author(s):  
J. Temple Black

Since its introduction by Fernandez-Moran, the diamond knife has gained wide spread usage as a common material for cutting of thin sections of biological and metallic materials into thin films for examination in the transmission electron microscope. With the development of high voltage E.M. and scanning transmission E.M., microtomy applications will become increasingly important in the preparation of specimens. For those who can afford it, the diamond knife will thus continue to be an important tool to accomplish this effort until a cheaper but equally strong and sharp tool is found to replace the diamond, glass not withstanding.In Figs. 1 thru 3, a first attempt was made to examine the edge of a used (β=45°) diamond knife by means of the scanning electron microscope. Because diamond is conductive, first examination was tried without any coating of the diamond. However, the contamination at the edge caused severe charging during imaging. Next, a thin layer of carbon was deposited but charging was still extensive at high magnification - high voltage settings. Finally, the knife was given a light coating of gold-palladium which eliminated the charging and allowed high magnification micrographs to be made with reasonable resolution.


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