In-Situ SEM Bulk Liquid Electrochemistry
| 1470 Series SEM | |
| Total Electrodes | 6 |
| True Reference Electrode | Yes* – drift rate less than 0.1 mV/min |
| True Counter Electrode | Yes* |
| Electrolytes | Aqueous, Wide range of organics |
| Spacer Range | 100 nm to 50 μm* |
| Heating Compatibility | Yes |
| SEM Compatibility | Custom integration |
How It Works
The scanning electron microscopy (SEM) bulk liquid electrochemistry specimen holder is the first and only in-situ liquid cell solution for SEM with capabilities allowing true reference and counter electrodes performance for electroanalytical measurements. The electrodes’ stability with little or no interference with the working electrodes allows superior performance and accuracy in the electroanalytical measurements.
The comparison of cyclic voltammetry – (current-voltage) data between a quasi electrochemistry system and our newest SEM bulk electrochemistry specimen holder shows the latter with distinct and consistent redox peaks over two cycles during electrodeposition of copper (Figure on the left). The quasi electrochemistry platform with unreal reference (e.g., metal) and unreal counter electrodes result in redox curves that do not have characteristic shapes, and peaks show artificial shifts during cycling. However, with the new SEM bulk electrochemistry holder, real reference electrodes such as Ag/AgCl (in KCl) and similar others are incorporated along with real counter electrodes (e.g., Pt). Our holder’s data show peaks that are distinct in shape, and no pseudo peak shift is observed during cycling, for the first time replicating in-situ what is observed in true bulk-scale electrochemical systems.
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Overview
Hummingbird Scientific’s dedicated SEM bulk liquid electrochemistry specimen holder, similar to the transmission electron microscopy (TEM) and X-ray Microscopy (XRM) counterparts, uses a real reference electrode (e.g., Ag/AgCl in KCl) and a real counter electrode (e.g., Pt) which allow the user to perform realistic in-situ electrochemistry that is for the first time quantitatively accurate and directly correlates to the industry-scale cells’ electrochemical behavior. This is vastly different from the conventional in-situ liquid cells that use pseudo reference electrodes which are unreliable and present inaccurate electrochemical data. Key characteristics of a new in-situ specimen holder include:
- Replication of electrochemical data to industry-scale cell
- Observation of transient electrochemical behavior in realtime.
Applications
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- Batteries
- Fuel cells
- Electrosynthesis
- Electrolysis
- Corrosion
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Multimodal Imaging
Along with the SEM system, our bulk liquid electrochemistry specimen holder is also available for transmission electron microscopy (TEM), and X-ray microscopy (XRM), as a full suite of multi-modal characterization techniques for materials at various length scales. The in-situ characterization made possible from the multi-modal platform provides complementary datasets suitable for accurate and reliable electroanalytical measurements of the sample at various length scales, and with complementary imaging and spectroscopy techniques.
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Accessories
Accessories available for your SEM liquid holder include:
- Bulk Reference Electrodes – Any Research Standard or User’s Choice
- Bulk Counter Electrodes – Any Research Standard or User’s Choice
- Specialized Liquid Electrochemistry Chips
- Custom SEM Seal-Checking Station
- Liquid-Heating Controller
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X-Ray/Synchrotron Liquid Holder See MoreHummingbird’s synchrotron holder is a complete in-situ x-ray lab system, enabling high-resolution material characterization in liquids. The system offers single-inlet, heating, electrochemical, spectroscopy, and cross-correlative features. |
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Operando liquid electrochemistry using graphene membrane working electrode
Researchers at EPFL published recent work characterizing graphene as a working electrode for CO2 electroreduction (CO2ER) of Cu nanocatalysts with the Hummingbird Scientific Generation V bulk liquid-electrochemical SEM system. The robust three-layer graphene membrane, which served as the sample carrier, working electrode, and liquid sealing membrane, was applied to the chip via a wet transfer process. Cyclic voltammetry (CV) plots indicated a wider inert cathodic range for the graphene working electrode than glassy carbon. Keeping the probe current low enabled imaging of nanocube degradation and secondary particle deposition during CO2ER at operating potential of -1.1 V vs RHE.
Figure: a) Schematic of graphene membrane preparation via wet transfer process. b) Cyclic voltammetry (CV) and chronoamperometry (CA) of SiNx, graphene, and glassy carbon comparing performance and inert potential range. c-d) Operando SEM, voltammetry and amperometry for CO2ER of Cu nanocatalysts.
Image Copyright © 2024 The Authors. Advanced Materials published by Wiley-VCH GmbH
Reference: Toleukhanova et. al. Adv. Mater. 36 (16) 2311133 (2024) DOI: 10.1021/acs.jpcc.0c09105
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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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| 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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