Identifying dynamic restructuring effects in nanocatalysts by combining in situ scanning transmission electron microscopy and in situ X-ray absorption spectroscopy: A review

Foucher, Alexandre C.; Stach, Eric A.

doi:10.1016/j.cattod.2023.114417

Cited by 4 publications

(2 citation statements)

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“…Stach and co-workers have pioneered technologies to bridge electrochemistry with liquid cell TEM 244 and provide a comprehensive review over its use in determining structural changes under reactive environments. 245 One minor drawback is the lower resolution due to the inherent properties of the cell. The use of liquid cell TEM was recently used by Zheng et al to study the mechanisms behind the growth of single platinum nanoparticles.…”

Section: Chemical Reviewsmentioning

confidence: 99%

“…We must caution the reader, however, and say that observations must be made under an electron beam, which may change electrocatalytic behavior. Stach and co-workers have pioneered technologies to bridge electrochemistry with liquid cell TEM and provide a comprehensive review over its use in determining structural changes under reactive environments …”

Section: Introduction To Single-entity Electrocatalytic Measurementsmentioning

confidence: 99%

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Single Entity Electrocatalysis

Clarke,

Krushinski,

Vannoy

et al. 2024

Chem. Rev.

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Making a measurement over millions of nanoparticles or exposed crystal facets seldom reports on reactivity of a single nanoparticle or facet, which may depart drastically from ensemble measurements. Within the past 30 years, science has moved toward studying the reactivity of single atoms, molecules, and nanoparticles, one at a time. This shift has been fueled by the realization that everything changes at the nanoscale, especially important industrially relevant properties like those important to electrocatalysis. Studying single nanoscale entities, however, is not trivial and has required the development of new measurement tools. This review explores a tale of the clever use of old and new measurement tools to study electrocatalysis at the single entity level. We explore in detail the complex interrelationship between measurement method, electrocatalytic material, and reaction of interest (e.g., carbon dioxide reduction, oxygen reduction, hydrazine oxidation, etc.). We end with our perspective on the future of single entity electrocatalysis with a key focus on what types of measurements present the greatest opportunity for fundamental discovery.

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Section: Chemical Reviewsmentioning

confidence: 99%

Section: Introduction To Single-entity Electrocatalytic Measurementsmentioning

confidence: 99%

Single Entity Electrocatalysis

Clarke,

Krushinski,

Vannoy

et al. 2024

Chem. Rev.

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Multimodal Insights of Regeneration Dynamics of Spent Bimetallic Catalysts by Full Field Hyperspectral Quick‐EXAFS Imaging and Environmental Transmission Electron Microscopy

Briois,

Nelayah,

La Fontaine

et al. 2024

ChemCatChem

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Multimodal measurements involving time‐resolved Ni and Cu K edges Quick‐EXAFS, time‐resolved hyperspectral Full Field quick‐EXAFS imaging with micrometer spatial resolution and aberration‐corrected Environmental Scanning Transmission Electron Microscopy have been performed over a NiCu catalyst used for the ethanol steam reforming reaction to establish structure‐activity relationships after regeneration. Activated catalysts are composed of 5‐10 nm monometallic nickel nanoparticles and 20 nm or larger bimetallic randomly alloyed NiCu nanoparticles. After 3h time on reactive stream, the monitoring of the regeneration of the coked deactivated catalyst at 500°C by Full Field hyperspectral XAS imaging evidences that the oxidative propagation front affects faster metallic Ni species than metallic Cu ones. This is ascribed to the presence of both NPs populations and to a restructuration of the alloyed bimetallic particles from a homogeneous solid solution towards a Ni‐rich shell upon oxygen adsorption. Furthermore, ESTEM characterization of the deactivated catalyst when passing from H2 to O2 atmosphere at 500°C for burning coke deposits evidences the fragmentation of the Ni and NiCu‐NPs driven by the Kirkendall effect in the encapsulated coked catalyst. The resulting increase of specific surface of active species is assumed to be responsible for the activity boost observed after regeneration.

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