In Situ Transmission Electron Microscopy of Electrocatalyst Materials: Proposed Workflows, Technical Advances, Challenges, and Lessons Learned.

IF 10.7 2区 材料科学 Q1 CHEMISTRY, PHYSICAL
Ahmed M Abdellah, Kholoud E Salem, Liza-Anastasia DiCecco, Fatma Ismail, Amirhossein Rakhsha, Kathryn Grandfield, Drew Higgins
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引用次数: 0

Abstract

In situ electrochemical liquid phase transmission electron microscopy (LP-TEM) measurements utilize micro-chip three-electrode cells with electron transparent silicon nitride windows that confine the liquid electrolyte. By imaging electrocatalysts deposited on micro-patterned electrodes, LP-TEM provides insight into morphological, phase structure, and compositional changes within electrocatalyst materials under electrochemical reaction conditions, which have practical implications on activity, selectivity, and durability. Despite LP-TEM capabilities becoming more accessible, in situ measurements under electrochemical reaction conditions remain non-trivial, with challenges including electron beam interactions with the electrolyte and electrode, the lack of well-defined experimental workflows, and difficulty interpreting particle behavior within a liquid. Herein a summary of the current state of LP-TEM technique capabilities alongside a discussion of the relevant experimental challenges researchers typically face, with a focus on in situ studies of electrochemical CO2 conversion catalysts is provided. A methodological approach for in situ LP-TEM measurements on CO2R catalysts prepared by electro-deposition, sputtering, or drop-casting is presented and include case studies where challenges and proposed workflows for each are highlighted. By providing a summary of LP-TEM technique capabilities and guidance for the measurements, the goal is for this paper to reduce barriers for researchers who are interested in utilizing LP-TEM characterization to answer their scientific questions.

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来源期刊
Small Methods
Small Methods Materials Science-General Materials Science
CiteScore
17.40
自引率
1.60%
发文量
347
期刊介绍: Small Methods is a multidisciplinary journal that publishes groundbreaking research on methods relevant to nano- and microscale research. It welcomes contributions from the fields of materials science, biomedical science, chemistry, and physics, showcasing the latest advancements in experimental techniques. With a notable 2022 Impact Factor of 12.4 (Journal Citation Reports, Clarivate Analytics, 2023), Small Methods is recognized for its significant impact on the scientific community. The online ISSN for Small Methods is 2366-9608.
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