|1470 Series SEM|
|True Reference Electrode||Yes*|
|True Counter Electrode||Yes*|
|Electrolytes||Aqueous, Wide range of organics|
|Spacer Range||100 nm to 2 um*|
|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.Edit
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.
- Fuel cells
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.Edit
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
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.0c09105Edit
Customization & Service
|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 and 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. The Journal of Physical Chemistry C (2020)||Abstract|