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Ferroelectrics, due to their polar nature and reversible switching, can be used to dynamically control surface chemistry for catalysis, chemical switching, and other applications such as water splitting. However, this is a complex phenomenon where ferroelectric domain orientation and switching are intimately linked to surface charges. In this work, the temperature‐induced domain behavior of ferroelectric‐ferroelastic domains in free‐standing BaTiO3 films under different gas environments, including vacuum and oxygen‐rich, is studied by in situ scanning transmission electron microscopy (STEM). An automated pathway to statistically disentangle and detect domain structure transformations using deep autoencoders, providing a pathway towards real‐time analysis is also established. These results show a clear difference in the temperature at which phase transition occurs and the domain behavior between various environments, with a peculiar domain reconfiguration at low temperatures, from a‐c to a‐a at ≈60 °C. The vacuum environment exhibits a rich domain structure, while under the oxidizing environment, the domain structure is largely suppressed. The direct visualization provided by in situ gas and heating STEM allows to investigate the influence of external variables such as gas, pressure, and temperature, on oxide surfaces in a dynamic manner, providing invaluable insights into the intricate surface‐screening mechanisms in ferroelectrics.
Ferroelectric surfaces can enable dynamic surface chemistry control due to their polar nature and reversible switching. This study investigates temperature‐induced domain behavior in free‐standing ferroelectric films under various gas environments using in situ scanning transmission electron microscopy and deep autoencoders. Real‐time analysis of domain structure under different environments provides invaluable insights into intricate surface‐screening mechanisms, responsible for surface chemistry control.