Experimental Requirements for High‐Temperature Solid‐State Electrochemical TEM Experiments

Author:

Ma Zhongtao1ORCID,Chatzichristodoulou Christodoulos1,Dacayan Waynah Lou1ORCID,Mølhave Kristian Speranza2ORCID,Chiabrera Francesco Maria13ORCID,Smitshuysen Thomas Erik Lyck2ORCID,Damsgaard Christian Danvad24ORCID,Simonsen Søren Bredmose1ORCID

Affiliation:

1. DTU Energy Fysikvej Kongens Lyngby 2800 Denmark

2. DTU Nanolab Ørsteds Plads Kongens Lyngby 2800 Denmark

3. Catalonia Institute for Energy Research (IREC) Jardins de les Dones de Negre 1, 2ª pl. Sant Adrià del Besòs Barcelona 08930 Spain

4. DTU Physics Fysikvej Kongens Lyngby 2800 Denmark

Abstract

AbstractThe 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. Particularly, the methodology of performing reliable electrochemical impedance spectroscopy measurements in reactive gases and at elevated temperatures for both single materials and solid oxide cells is described. The presented results include impedance measurements of electronic conductors, an ionic conductor, and a mixed ionic and electronic conductor, all materials typically applied in solid oxide fuel and electrolysis cells. It is shown that how TEM and impedance spectroscopy can be synergically integrated to measure the transport and surface exchange properties of materials with nanoscale dimensions and to visualize their structural and elemental evolution via TEM/STEM imaging and spectroscopy.

Funder

European Research Council

Publisher

Wiley

Subject

General Materials Science,General Chemistry

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