Experimental Requirements for High-Temperature Solid-State Electrochemical TEM Experiments.

The ability to perform both electrochemical and structural/elemental characterization in the same experiment and at the nanoscale allows to directly link electrochemical performance to the material properties and their evolution over time and operating conditions. Such experiments can be important for the further development of solid oxide cells, solid-state batteries, thermal electrical devices, and other solid-state electrochemical devices. The experimental requirements for conducting solid-state electrochemical TEM experiments in general, including sample preparation, electrochemical measurements, failure factors, and possibilities for optimization, are presented and discussed.

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 (O and H /H O), 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.