In-Situ SEM Bulk Liquid Electrochemistry

Introducing the world's first bulk liquid-electrochemistry SEM holder

Technical Specs

1470 Series SEM
Total Electrodes 6
True Reference Electrode  Yes*
True Counter Electrode Yes*
Electrolytes  Aqueous, Wide range of organics
Spacer Range  100 nm to 2 um*
Heating Compatibility Yes
SEM Compatibility Custom integration

* Different Configurations and Materials Available

Features

Featured Research

Quantitatively tracking electrodeposition of catalyst particles in SEM in real-time

Researchers at the Fritz-Haber Institute of the Max Planck Society used Hummingbird’s bulk liquid electrochemistry specimen holder in the SEM to demonstrate an accurate and consistent way to deposit copper oxide catalysts in various shapes and sizes. The study made use of the reliable reference electrode system incorporated in the bulk liquid system to quantitatively track the electrodeposited copper cubes with different facets and sizes over many (repeatable) cycles. For example, the growth starts from nucleation during the first cycle and deposition and dissolution of selective crystals occurs in the third and subsequent cycles. The work provides critical insights into developing catalysts to convert carbon dioxide into useful chemicals and fuels.

Figure: Current-voltage curve tracking oxidation and reduction peaks of copper oxide in different concentrations of KCl solution in 5 mM copper sulfate. Growth of Cu cubes and generation/dissolution of noncubic particles.

Image Copyright © 2021 American Chemical Society

Reference: Grosse et al. J. Phys. Chem. C 2020, 124, 49, 26908–26915.  DOI: 10.1021/acs.jpcc.0c09105

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Video Spotlight

In-situ  SEM showing nucleation and growth of Cu cubes during electrochemical cycling

The video on the left published by researchers at Fritz-Haber Institute of the Max Planck Society shows the control nucleation and growth of Cu cubes during a potential sweep. The shape and size of the cubes’ growth correspond with the number of cycles.  The result demonstrates that the growth of particles such as Cu cubes can be accurately tuned to achieve optimal sizes and shapes as required for a particular application such as catalysis.

The accuracy in the electrosynthesis of nanoparticles directly correlates to the reliability and accuracy of reference electrodes used over multiple (repeatable) cycles and cannot be achieved with a quasi electrochemistry platform with unrealistic/pseudo reference electrodes.

Video Copyright © 2021 American Chemical Society

Reference: Grosse et al. J. Phys. Chem. C 2020, 124, 49, 26908–26915. DOI: 10.1021/acs.jpcc.0c09105

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Customization & Service

Selected Publications

Saltanat Toleukhanova, Tzu-Hsien Shen, Chen Chang, Swathilakshmi Swathilakshmi, Tecla Bottinelli Montandon, and Vasiliki Tileli. “Graphene Electrode for Studying CO2 Electroreduction Nanocatalysts under Realistic Conditions in Microcells.” Adv. Mater. (2024) Abstract
Aram Yoon, Antonia Herzog, Philipp Grosse, Daan Hein Alsem, See Wee Chee, and Beatriz Roldán Cuenya. “Dynamic Imaging of Nanostructures in an Electrolyte with a Scanning Electron Microscope.” Microscopy & Microanalysis (2021) Abstract
Philipp Grosse, Aram Yoon, Clara Rettenmaier, See Wee Chee, and Beatriz Roldan Cuenya. “Growth Dynamics and Processes Governing the Stability of Electrodeposited Size-Controlled Cubic Cu Catalysts.” J. Phys. Chem. C (2020) Abstract
See Wee Chee, Aram Yoon, Rosa Aran-Ais, Ruben Rizo, Philipp Grosse, and Beatriz Roldan Cuenya. “Investigating the Behavior of Cu-based Catalysts During Electrochemical CO2 Reduction with Liquid Cell Electron Microscopy.” Microscopy & Microanalysis (2020) Abstract

 

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