Best practices for in-situ and operando techniques within electrocatalytic systems

Prajapati, Aditya; Hahn, Christopher; Weidinger, Inez M.; Shi, Yanmei; Lee, Yonghyuk; Alexandrova, Anastassia N.; Thompson, David; Bare, Simon R.; Chen, Shuai; Yan, Shuai; Kornienko, Nikolay

doi:10.1038/s41467-025-57563-6

Title: Best practices for in-situ and operando techniques within electrocatalytic systems

Journal Article · 16 March 2025 · Nature Communications

DOI: https://doi.org/10.1038/s41467-025-57563-6 · OSTI ID:2539990

Prajapati, Aditya ^[1];

^[1];

^[2];

^[3]; Lee, Yonghyuk ^[4];

^[4]; Thompson, David ^[5];

^[6];

^[7]; Yan, Shuai ^[7];

^[7]

Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States)
Technische Universität Dresden (Germany)
Tianjin Univ. (China)
Univ. of California, Los Angeles, CA (United States)
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL); Univ. of Arkansas, Fayetteville, AR (United States)
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)
Univ. of Bonn (Germany)

In-situ and operando techniques in heterogeneous electrocatalysis are a powerful tool used to elucidate reaction mechanisms. Ultimately, they are key in determining concrete links between a catalyst’s physical/electronic structure and its activity en route to designing next-generation systems. To this end, the exact execution and interpretation of these lines of experiments is critical as this determines the strength of conclusions that can be drawn and what uncertainties remain. Instead of focusing on how techniques were used to understand systems, as is the case with most reviews on the topic, this work instead initiates a nuanced discussion of 1) how to best carry out each technique and 2) initiate a nuanced analysis of which level of insights can be drawn from the set of in-situ or operando experiments/controls carried out. We focus on several commonly used techniques, including vibrational (IR, Raman) spectroscopy, X-ray absorption spectroscopy and electrochemical mass spectrometry. In addition to this, we include sections of reactor design and the link with theoretical modelling that are applicable across all techniques. While we focus on heterogeneous electrocatalysis, we make links when appropriate to the areas of photo- and thermo-catalytic systems. We highlight common pitfalls in the field, how to avoid them, and what sets of complementary experiments may be used to strengthen the analysis. We end with an overview of what gaps remain in in-situ and operando techniques and what innovations must be made to overcome them.

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Research Organization:: Energy Frontier Research Centers (EFRC) (United States). Center for Closing the Carbon Cycle; Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States)

Sponsoring Organization:: German Research Foundation (DFG); National Natural Science Foundation of China (NSFC); USDOE National Nuclear Security Administration (NNSA); USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB)

Grant/Contract Number:: AC52-07NA27344; SC0019152; SC0023427

OSTI ID:: 2539990

Report Number(s):: LLNL--JRNL-868780; 1105078

Journal Information:: Nature Communications, Journal Name: Nature Communications Journal Issue: 1 Vol. 16; ISSN 2041-1723

Publisher:: Nature Publishing GroupCopyright Statement

Country of Publication:: United States

Language:: English

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