Local temperature measurement in TEM by parallel beam electron diffraction

Abstract

With the recent advances in instrumentation pushing the limits of in situ transmission electron microscopy, the question of local sample temperature comes into focus again. In this work the applicability of parallel beam electron diffraction to locally measure and monitor the sample temperature in TEM is assessed, with applications for in situ heating experiments in mind. With Au nanoparticles applied to the sample surface, temperature is measured in the range from RT to 890°C by evaluating the change in scattering angle upon thermal expansion. Repeated measurements at constant temperature reveal a statistical precision of the method as good as 2.8K. The applicability to locally measure the temperature is demonstrated mapping the temperature gradient across a heating chip. Owing to instantaneous response of thermal expansion to temperature changes, the method is well suited for monitoring even quick temperature changes, as demonstrated by quenching experiments. In order to enable extensive in situ studies, an evaluation method capable of processing large datasets with high precision is developed. Beam parallelity is identified as crucial experimental prerequisite and a routine is established, optimizing the microscope alignment in terms of beam parallelity. Apart from establishing a procedure for local temperature measurement, the present work demonstrates the unique capabilities of MEMS-based in situ heating equipment.

Keywords: Beam parallelity; In situ microscopy; Metallic nanoparticles; Microscope alignment; Temperature measurement; Transmission electron microscopy.