Electrochemical Impedance Spectroscopy Integrated with Environmental Transmission Electron Microscopy

The concept of combining electrical impedance spectroscopy (EIS) with environmental transmission electron microscopy (ETEM) is demonstrated by testing a specially designed micro gadolinia-doped ceria (CGO) sample in reactive gasses (O₂ and H₂/H₂O), at elevated temperatures (room temperature—800 °C) and with applied electrical potentials. The EIS-TEM method provides structural and compositional information with direct correlation to the electrochemical performance. It is demonstrated that reliable EIS measurements can be achieved in the TEM for a sample with nanoscale dimensions. Specifically, the ionic and electronic conductivity, the surface exchange resistivity, and the volume-specific chemical capacitance are in good agreement with results from more standardized electrochemical tests on macroscopic samples. CGO is chosen as a test material due to its relevance for solid oxide electrochemical reactions where its electrochemical performance depends on temperature and gas environment. As expected, the results show increased conductivity and lower surface exchange resistance in H₂/H₂O gas mixtures where the oxygen partial pressure is low compared to experiments in pure O₂. The developed EIS-TEM platform is an important tool in promoting the understanding of nanoscale processes for green energy technologies, e.g., solid oxide electrolysis/fuel cells, batteries, thermoelectric devices, etc.