Proceedings of MATSUS Spring 2024 Conference (MATSUS24)
DOI: https://doi.org/10.29363/nanoge.matsus.2024.283
Publication date: 18th December 2023
In-situ techniques play an important role in gaining real-time insights into dynamic processes at the nanoscale. Employing a specialized TEM holder and chips, the electrochemical TEM (EC-TEM) setup allows for the direct observation of (nano)materials undergoing electrochemical reactions within their confined environments. This dynamic characterization enables the tracking of structural changes, such as phase transformations and morphological evolution.[1,2] In our research, we studied the electrochemical growth of Cu on a GC electrode, as a model system.
While the in-situ characterization offers a new avenue of opportunities, it also comes with specific challenges that we need to overcome, such as the confined environment of the EC-TEM holder, and the beam-related effect. Moreover, nucleation and growth are especially sensible to the surface state, which can end up in the formation of different structures. To consider this, we conducted a detailed analysis of the GC working electrode situated on the specialized TEM chip surface using a scanning probe technique, Scanning Electrochemical Cell Microscopy (SECCM). This technique allowed us to characterize the GC electrochemical activity within a few micrometers, which, for the case of GC, have been shown before to be heterogenous.[1,3] Overall, performing an extensive characterization of the electrochemical response of the TEM chips, in both in-situ and ex-situ conditions, allows us to better understand the electrochemical processes under TEM imaging conditions. In the context of our work, this is of special interest for the better understanding the fundamentals of metal nucleation, growth and dissolution on/from glassy carbon electrodes. This knowledge is essential for the rationalized design of active and durable nanostructured electrocatalysts for a wide range of electrochemical energy conversion and storage technologies.
I would like to express my sincere gratitude to the Fund for Scientific Research - Flanders (FWO), under contract G0C3121N, for supporting this research.
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