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

Research output: Contribution to journal › Review article › Contributed › peer-review

Contributors

  • Aditya Prajapati - , Lawrence Livermore National Laboratory (Author)
  • Christopher Hahn - , Lawrence Livermore National Laboratory (Author)
  • Inez M. Weidinger - , Chair of Electrochemistry (Author)
  • Yanmei Shi - , Tianjin University (Author)
  • Yonghyuk Lee - , University of California at Los Angeles (Author)
  • Anastassia N. Alexandrova - , University of California at Los Angeles (Author)
  • David Thompson - , Stanford University, University of Arkansas System (Author)
  • Simon R. Bare - , Stanford University (Author)
  • Shuai Chen - , University of Bonn (Author)
  • Shuai Yan - , University of Bonn (Author)
  • Nikolay Kornienko - , University of Bonn (Author)

Abstract

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.

Details

Original languageEnglish
Article number2593
JournalNature communications
Volume16
Issue number1
Publication statusPublished - 16 Mar 2025
Peer-reviewedYes

External IDs

PubMed 40091111