The microstructure of polymers controls their chemical reactivity as well as their mechanical and transport properties. However, quantitative characterization of the microstructure of soft polymers is not often possible or practical with the few analytical methods available to study it at the sub-micrometer scale. Freeze-fracturing is one such method, but often the surfaces of samples prepared with the process are too rough, leaving only a very small area appropriate for quantitative SEM investigation.
The results demonstrate that cryo-BIB-SEM enables microstructure characterization of soft polymers with high resolution over large planar areas of damage-free sample cross sections. Only minor artifacts from the cryo-BIB-SEM sample preparation process were seen at the scale of observation, none of which appear to be a consequence of freezing.
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