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Potential-Dependent Morphology of Copper Catalysts During CO₂ Electroreduction Revealed by In?Situ Atomic Force Microscopy.

ABSTRACT: Electrochemical AFM is a powerful tool for the real-space characterization of catalysts under realistic electrochemical CO₂ reduction (CO₂ RR) conditions. The evolution of structural features ranging from the micrometer to the atomic scale could be resolved during CO₂ RR. Using Cu(100) as model surface, distinct nanoscale surface morphologies and their potential-dependent transformations from granular to smoothly curved mound-pit surfaces or structures with rectangular terraces are revealed during CO₂ RR in 0.1?m KHCO₃ . The density of undercoordinated copper sites during CO₂ RR is shown to increase with decreasing potential. In?situ atomic-scale imaging reveals specific adsorption occurring at distinct cathodic potentials impacting the observed catalyst structure. These results show the complex interrelation of the morphology, structure, defect density, applied potential, and electrolyte in copper CO₂ RR catalysts.

SUBMITTER: Simon GH

PROVIDER: S-EPMC7898873 | biostudies-literature | 2021 Feb

REPOSITORIES: biostudies-literature

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Potential-Dependent Morphology of Copper Catalysts During CO2 Electroreduction Revealed by In Situ Atomic Force Microscopy.

Simon Georg H GH Kley Christopher S CS Roldan Cuenya Beatriz B

Angewandte Chemie (International ed. in English) 20201201 5

Electrochemical AFM is a powerful tool for the real-space characterization of catalysts under realistic electrochemical CO2 reduction (CO2 RR) conditions. The evolution of structural features ranging from the micrometer to the atomic scale could be resolved during CO2 RR. Using Cu(100) as model surface, distinct nanoscale surface morphologies and their potential-dependent transformations from granular to smoothly curved mound-pit surfaces or structures with recta ...[more]

PMID: 33035401

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Project description:Using a combination of in situ bulk and surface characterization techniques, we provide atomic-scale insight into the complex surface and bulk dynamics of a LaNiO3 perovskite material during heating in vacuo. Driven by the outstanding activity LaNiO3 in the methane dry reforming reaction (DRM), attributable to the decomposition of LaNiO3 during DRM operation into a Ni//La2O3 composite, we reveal the Ni exsolution dynamics both on a local and global scale by in situ electron microscopy, in situ X-ray diffraction and in situ X-ray photoelectron spectroscopy. To reduce the complexity and disentangle thermal from self-activation and reaction-induced effects, we embarked on a heating experiment in vacuo under comparable experimental conditions in all methods. Associated with the Ni exsolution, the remaining perovskite grains suffer a drastic shrinkage of the grain volume and compression of the structure. Ni particles mainly evolve at grain boundaries and stacking faults. Sophisticated structure analysis of the elemental composition by electron-energy loss mapping allows us to disentangle the distribution of the different structures resulting from LaNiO3 decomposition on a local scale. Important for explaining the DRM activity, our results indicate that most of the Ni moieties are oxidized and that the formation of NiO occurs preferentially at grain edges, resulting from the reaction of the exsolved Ni particles with oxygen released from the perovskite lattice during decomposition via a spillover process from the perovskite to the Ni particles. Correlating electron microscopy and X-ray diffraction data allows us to establish a sequential two-step process in the decomposition of LaNiO3 via a Ruddlesden-Popper La2NiO4 intermediate structure. Exemplified for the archetypical LaNiO3 perovskite material, our results underscore the importance of focusing on both surface and bulk characterization for a thorough understanding of the catalyst dynamics and set the stage for a generalized concept in the understanding of state-of-the art catalyst materials on an atomic level.

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Potential-Dependent Morphology of Copper Catalysts During CO₂ Electroreduction Revealed by In?Situ Atomic Force Microscopy.

Publications

Potential-Dependent Morphology of Copper Catalysts During CO<sub>2</sub> Electroreduction Revealed by In Situ Atomic Force Microscopy.

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Dataset Information

Potential-Dependent Morphology of Copper Catalysts During CO2 Electroreduction Revealed by In?Situ Atomic Force Microscopy.

Publications

Potential-Dependent Morphology of Copper Catalysts During CO<sub>2</sub> Electroreduction Revealed by In Situ Atomic Force Microscopy.

Similar Datasets

OmicsDI is part of the ELIXIR infrastructure

Tweets

Potential-Dependent Morphology of Copper Catalysts During CO₂ Electroreduction Revealed by In?Situ Atomic Force Microscopy.