In Situ Transmission Electron Microscopy Solutions for Real-World Applications— Advances in Operando Methods for the Study of Temperature-dependent Electrochemical Processes

Effective solutions for addressing a myriad of critical issues such as clean energy production, pollutant remediation, drug efficacy, and computing performance are contingent on development of new, high-performance, functional materials. Effective exploitation of the structure-function relationships that control a material’s performance requires a robust understanding of the mechanistic pathways and transient intermediate structures responsible for its behavior. In-situ and/or operando transmission electron microscopy (TEM) techniques enables researchers to follow a materials’ morphological changes in real-time under its native working conditions [1-3].

Over the course of the last twenty years these studies have spanned a wide range of application spaces from basic beam-assisted nanoparticle growth [4] to complex heterogeneous catalysis processes [REF]. In order for these studies to advance further, and lead to meaningful solutions in the real-world, in-situ TEM tools including hardware, MEMs-based sample supports, experimental workflows and data analysis processes must be tailored to real-world applications and integrated with complementary, correlative benchtop and other in-situ techniques to generate relevant, actionable data.

Here we present examples of holistic approaches used to optimize in-situ TEM workflows for battery and electrocatalysis applications and mitigate the most common challenges associated with operando liquid-EM electrochemical studies, including development a next-generation liquid-TEM system specifically optimized for energy materials research. With a working temperature range of-50 °C to 300 °C in-situ electrochemical experiments can now be performed under conditions that accurately replicate a real-world working environment. Combined with better flow performance, integration of conventional reference electrode materials, and machine-vision data integration and analysis software, in-situ TEM workflows for electrochemical studies can now generate more robust and actionable data sets for a better understanding of the critical factors required to optimize material properties

[1] Pu, S.D. et al. (2020) ACS Energy Letters, 5, 2283–2290.
[2] Balaghi, S.E. et al. (2021) ACS Applied Materials & Interfaces, 13, 19927–19937.
[3] Yang, Y. et al. (2023) Nature, 614, 262-270
[4] Kim, et al., MRS Bulletin (2024) 49, 365–376
[5] Chee, S.W et al., Chemical Reviews 2023 123 (23), 13374-13418