Cathode structures derived from carbonized electrospun polyacrylonitrile (PAN) nanofibers are a current line of development for improvement of gas diffusion electrodes for metal-air batteries and fuel cells. Diameter, surface morphology, carbon structure and chemical composition of the carbon based fibers play a crucial role for the functionality of the resulting cathodes, especially with respect to oxygen adsorption properties, electrolyte wetting and electronic conductivity. These functionalities of the carbon fibers are strongly influenced by the carbonization process. Hitherto, fibers were mostly characterized by ex situ methods, which require great effort for statistical analysis in the case of microscopy. Here, we show the morphological and structural evolution of nanofibers during their carbonization at up to 1000 °C by in situ transmission electron microscopy (TEM). Changes in fiber diameter and surface morphology of individual nanofibers were observed at 250 °C, 600 °C, 800 °C and 1000 °C in imaging mode. The structural evolution was studied by concomitant high resolution TEM and electron diffraction. The results show with comparatively little effort shrinkage of the nanofiber diameter, roughening of the surface morphology and formation of turbostratic carbon with increasing carbonization temperature at identical locations.
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