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Small (Weinheim an der Bergstrasse, Germany)
Jul, 2021;17 (27): e2004289.

Operando Surface Spectroscopy and Microscopy during Catalytic Reactions: From Clusters via Nanoparticles to Meso-Scale Aggregates.

Günther Rupprechter
Author Information
  1. Günther Rupprechter: Institute of Materials Chemistry, Technische Universität Wien, Getreidemarkt 9/BC/01, Vienna, 1060, Austria. ORCID
PMID: 33694320 DOI: 10.1002/smll.202004289

Abstract

Operando characterization of working catalysts, requiring per definitionem the simultaneous measurement of catalytic performance, is crucial to identify the relevant catalyst structure, composition and adsorbed species. Frequently applied operando techniques are discussed, including X-ray absorption spectroscopy, near ambient pressure X-ray photoelectron spectroscopy and infrared spectroscopy. In contrast to these area-averaging spectroscopies, operando surface microscopy by photoemission electron microscopy delivers spatially-resolved data, directly visualizing catalyst heterogeneity. For thorough interpretation, the experimental results should be complemented by density functional theory. The operando approach enables to identify changes of cluster/nanoparticle structure and composition during ongoing catalytic reactions and reveal how molecules interact with surfaces and interfaces. The case studies cover the length-scales from clusters via nanoparticles to meso-scale aggregates, and demonstrate the benefits of specific operando methods. Restructuring, ligand/atom mobility, and surface composition alterations during the reaction may have pronounced effects on activity and selectivity. The nanoscale metal/oxide interface steers catalytic performance via a long ranging effect. Combining operando spectroscopy with switching gas feeds or concentration-modulation provides further mechanistic insights. The obtained fundamental understanding is a prerequisite for improving catalytic performance and for rational design.

Keywords

clusters heterogeneous catalysis interfaces nanoparticles operando surface science

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Grants

  1. F4502/04-N16/Austrian Science Fund
  2. W1243/Austrian Science Fund
  3. I942-N17/Austrian Science Fund
  4. I1041-N28/Austrian Science Fund
  5. P 32772-N/Austrian Science Fund
  6. I 4434-N/Austrian Science Fund
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