Three-dimensional nanostructure analysis of non-stained Nafion in fuel-cell electrode by combined ADF-STEM tomography

The polymer electrolyte fuel cell (PEFC) is one of the strongest candidates for a next-generation power source for vehicles which do not emit CO2 gas as exhaust gas. The key factor in PEFCs is the nano-scaled electrochemical reactions that take place on the catalyst material and an ionomer supported by a carbon support. However, because the nano-scaled morphological features of the key materials in the catalyst compound cannot be observed clearly by transmission electron microscopy, improvement of PEFC performance had been approached by an imaginal schematic diagram based on an electrochemical analysis. In this study, we revealed the nano-scaled morphological features of the PEFC electrode in three dimensions and performed a quantitative analysis of the nanostructure by the newly developed 'Combined ADF-STEM tomography technique'. This method combines information from plural annular darkfield detectors with different electron collection angles and can emphasize the difference of the electron scattering intensity between the ionomer and carbon in the cross-sectional image of the reconstructed three-dimensional (3D) data. Therefore, this segmentation method utilizing image contrast does not require a high electron beam current like that used in energy dispersive X-ray analysis, and thus is suitable for electron beam damage-sensitive materials. By eliminating the process of manually determining the thresholds for obtaining classified component data from grayscale data, the obtained 3D structures have sufficient accuracy to allow quantitative analysis and specify the nano-scaled structural parameters directly related to power generation characteristics.