Abstract
The study of in situ or operando electrochemistry entails observing electrochemical behavior of samples in environments as close to “real working conditions” as possible. Scanning/transmission electron microscopy (S/TEM) enables researchers to characterize physical behavior on the sub-nanometer scale, but conventional S/TEM techniques require sample imaging and analysis in a high-vacuum environment. Recent advances in sample holder technology for S/TEM – specifically, the introduction of closed-cell S/TEM holders and the development of MEMS-based sample supports – have overcome this limitation. Closed-cell holders allow researchers to study their electrochemical systems in liquid, including the option to flow or exchange electrolyte across the sample, by hermetically sealing the experiment from the high-vacuum environment of the S/TEM column. MEMS-based sample supports with integrated electrodes, thin membrane windows, and controlled flow of electrolyte allow researchers to apply electrical stimuli while imaging. Together, these technologies allow the direct observation of processes at the nanoscale that influence material performance, such as the formation of the solid electrolyte interphase (SEI) layer during lithium-ion battery cycling [1], the preferential corrosion of stainless steel at sulfite [2] and silicate [3] inclusions, and the dynamic evolution of shape-controlled nanocrystals for CO2 reduction [4-6]. Understanding the structure-function relationship of these materials at the nanoscale facilitates the efficient innovation of new materials that are more functional, cost-efficient, and environmentally friendly.In this presentation, we will share initial results from the next generation of in situ electrochemistry systems, pushing closer to “real working conditions” through advanced temperature control of the electrode-electrolyte interface. Many applications require increased temperatures, including research on fuel cell catalysts and corrosion. We will discuss the kinetics of well-known redox couples (Figure 1a) and of dendrite formation (Figure 1b) as a function of the temperature at the anode surface, the different spectroscopic techniques available when in situ electrochemistry is coupled with electron microscopy, and the implications of this new technology to research across numerous application fields including fuel cells, ionic liquids, batteries, corrosion, and electrocatalysis.[1] W. Dachraoui, et al. ACS Nano 2023 17(20), 20434-20444[2] D. Kovalov, et al. Corros. Sci. 2022 199, 110184[3] M. Tian, et al. Corros. Sci. 2022 208, 110659[4] Y. Yang, et al. Nature 2023 614, 262-270[5] Y. Yang, et al. J. Am. Chem. Soc. 2022 144(34), 15698-15708[6] A.M. Abdellah, et al. Nat. Commun. 2024 15, 938 Figure 1
Published Version
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