Cross-sectional observation of nanostructured catalyst layer of polymer electrolyte fuel cell using FIB/SEM

The catalyst layer structure of a membrane electrode assembly (MEA) affects fuel cell performance. Cross-sectional observation is the most simple and effective way to evaluate the catalyst layer structure. Although focused ion beam (FIB) is a common tool for cross-sectional observation, sputtering of the ion beam causes heat damage to the MEA sample, which in previous studies was mitigated by sample cooling using liquid nitrogen. In this study, the sample holder and FIB stage were newly developed for cross-sectional observation of MEA catalyst layers, which suppressed heat damage by thermoelectric cooling using Peltier elements. Two types of degradation mode tests, load cycle and startup-shutdown cycle, were conducted on the MEA sample and their cross-sectional observations were performed using newly developed scanning electron microscope stages, which can mount the sample holder directly. The growth of platinum nanoparticles corresponding to the degradation of the active surface area was clearly observed for the sample subjected to the load cycle test. On the other hand, the corrosion of carbon particles was observed for the startup-shutdown sample. Since the cross-sectional samples were fabricated without heat damage by FIB with the newly developed stage, the difference in microstructure for these modes could be clearly distinguished. •Cross-sectional observation techniques without heat damages for MEA were developed.•Growth of platinum nanoparticles was observed for the load cycle sample.•Corrosion of carbon particles was observed for the startup–shutdown sample.