Optimization of permanganic etching of polyethylenes for scanning electron microscopy

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Abstract
The permanganic etching technique has been studied as a function of time, temperature, and concentration for a series of polyethylenes. Kinetic studies show that a film of reaction products builds up on the surface, impeding further etching, an effect which is greatest for the lowest‐crystallinity polymers. SEM studies combined with EDS show that the film contains sulfur, potassium, and some manganese. An artifact is produced by the etching process which is impossible to remove by washing procedures if certain limits of time, temperature, and concentration are exceeded. For lower‐crystallinity polyethylenes multiple etching and washing steps were required for optimal resolution. Plastic deformation during specimen preparation, whether from scratches or freeze fracturing, enhances artifact formation. When appropriate procedures are used virtually artifact‐free surfaces can be produced allowing a combination of permanganic etching and scanning electron microscopy to give a rapid method for detailed morphological characterization of bulk specimens.

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