Nanoscale temperature measurement during temperature controlled in situ TEM using Al plasmon nanothermometry

Over recent years, the advent of microelectromechanical system (MEMS)-type microheaters has pushed the limits of temperature controlled in situ transmission electron microscopy (TEM). In particular, by enabling the observation of the structure of materials in their application environments, temperature controlled TEM provides unprecedented insights into the link between the properties of materials and their structure in real-world problems, a clear knowledge of which is necessary for rational development of functional materials with new or improved properties. While temperature is the key parameter in such experiments, accessing the precise temperature of the sample at the nanoscale during observations still remains challenging. In the present work, we have applied aluminium plasmon nanothermometry technique that monitors the temperature dependence of the volume plasmon of Al nanospheres using electron energy loss spectroscopy for in situ local temperature determination over MEMS-type microheaters. With access to local temperatures between room temperature to 550 ^∘C, we have assessed the spatial and temporal stabilities of these microheaters when they operate at different setpoint temperatures both under vacuum and in the presence of a static H₂ gas environment. Temperature comparisons performed under the two environments show discrepancies between local and setpoint temperatures.