Name: SEM Bulk Liquid Electrochemistry
Brand: Hummingbird Scientific

Perform liquid-phase electrochemistry inside your SEM with electrochemical performance that closely matches conventional bulk benchtop measurements

True Bulk Electrochemistry Inside the SEM

The Hummingbird Scientific SEM Bulk Liquid Electrochemistry Sample Holder is the first in-situ liquid-phase SEM platform designed to reproduce true bulk electrochemical behavior inside the SEM. Unlike conventional liquid-cell SEM systems that rely on patterned on-chip electrodes, it incorporates off-chip bulk reference and counter electrodes to deliver electrochemical measurements that closely match benchtop experiments while enabling simultaneous nanoscale imaging.

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Designed for Advanced Electrochemistry Research

Ideal for researchers studying liquid-phase electrochemical processes in batteries, electrocatalysts, and energy materials, where direct observation of reaction mechanisms and material evolution at the nanoscale is critical.

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Understand What Drives Electrochemical Performance

Electrochemical measurements alone often cannot reveal why materials succeed, degrade, or fail. The holder is optimized for versatility in SEM environments with multiple unique detectors including scattered (BSE and SE) and transmission (STEM) oriented around the sample stage inside of an evacuated chamber. By directly correlating electrochemical data with real-time nanoscale observations, researchers can uncover reaction pathways, structural transformations, and degradation mechanisms that govern material behavior, accelerating the development of next-generation energy and electrochemical technologies.

SEM Bulk Liquid Electrochemistry Sample Holder

Hummingbird Advantages:

Replicates benchtop electrochemical measurements inside the SEM.
Eliminates signal drift and instability associated with on-chip pseudo-reference electrodes.
Supports quantitative cyclic voltammetry, chronoamperometry, battery cycling, corrosion studies, and electrocatalysis.
Correlates electrochemical data with real-time nanoscale imaging of material transformations and degradation mechanisms.
Features screw-free liquid-cell assembly with self-aligning windows for fast, reproducible sample loading.
Compatible with SEM, TEM, and X-ray microscopy workflows using cross-platform microfabricated chips.

Technical Specs

1470 Series SEM

Total Electrodes

6

True Reference Electrode

Yes

True Counter Electrode

Yes

Counter Electrode Material

User’s choice of material

Electrolytes

Aqueous and a wide range of organic solvents

Spacer Range

100 nm to 50 μm

Heating Capability

Yes

SEM Compatibility

Custom integration

Available For:

Conventional In-Situ Liquid-Cell Electrochemistry vs Bulk In-Situ Liquid-Cell Electrochemistry

Conventional in-situ liquid-cell electrochemistry uses patterned on-chip electrodes that can introduce limitations in electrochemical fidelity, cycling stability, and correlation with conventional benchtop electrochemistry. In contrast, our bulk liquid-cell electrochemistry architecture uses off-chip bulk reference and counter electrodes to enable quantitative electrochemical measurements and simultaneous nanoscale imaging inside TEM, SEM, and X-ray microscopes.

Feature

Conventional Liquid-Cell Electrochemistry with On-Chip Electrodes

Bulk Liquid-Cell Electrochemistry with Off-Chip Electrodes

Electrode Architecture

Microfabricated on-chip reference and counter electrodes, which are constrained by chip geometry, thin film degradation, and have limited material options.

True off-chip bulk reference and counter electrodes with larger geometries and flexible material selection.

Electrochemical Fidelity

Electrochemical behavior often differs from conventional benchtop measurements, with electrochemical curves showing shifted peak positions and altered shapes.

Electrochemical behavior closely matches conventional benchtop measurements, with electrochemical curves exhibiting similar shapes and matching peak locations.

Imaging fidelity

Some negative applied voltages can induce a water splitting environment near the counter electrode surface. With an on-chip counter electrode, this results in H₂ bubble formation which can impede liquid-cell imaging.

With the counter electrode relocated far from the viewing area, the in-situ electrochemistry experiment can be conducted with no affect of bubbles in the region of interest for characterization.

Cycling Stability

Repeated current-voltage cycling can cause electrode degradation, signal drift, and reduced reproducibility.

Bulk electrodes provide stable, repeatable electrochemical measurements during extended cycling experiments.

Best Suited For

Qualitative or semi-qualitative liquid-cell electrochemical studies.

Quantitative in-situ and operando electrochemical studies.

How it Works

The SEM Bulk Liquid Electrochemistry Sample Holder integrates a sealed microfluidic liquid cell with true bulk reference and counter electrodes positioned off-chip, enabling accurate electrochemical control within the SEM. Real reference electrodes (e.g., Ag/AgCl) provide stable potentials, while bulk counter electrodes (e.g., Pt) support consistent current flow, eliminating the instability and drift common in on-chip systems.

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During operation, electrolyte flows through the liquid cell while electrochemical cycling is performed on the working electrode under direct electron beam observation. This architecture decouples electrochemical performance from geometric and material limitations of on-chip microfabricated electrodes, delivering reproducible current voltage responses with well-defined redox peaks closely matching bulk electroanalytical behavior while simultaneously enabling nanometer resolution imaging in liquid environments.

Key Features and Capabilities

Built for Diverse Research Applications

Battery Materials

Directly visualize battery cycling, ion transport, dendrite formation, interface evolution, and structural changes.

Charge-Discharge Cycling

Bio/Soft Materials

Visualize biological and soft matter systems dynamics, including growth, interactions, and degradation.

Biomineralization

Self-Assembly Processes

Metal-Organic Framework Dynamics

Soft Matter Dynamics

Biomolecular Interactions

Catalysis

Directly observe the mechanisms that drive catalyst activity, selectivity, and degradation.

Heterogeneous Catalysis

Structure-Performance Relationship

Catalyst Structural Transformations

Catalyst Chemical Transformations

Catalyst Redox

Electrochemistry

Study electrodeposition, electrocatalysis, corrosion mechanisms, and electrochemical interface evolution.

Cyclic Voltammetry (CV)

Linear Sweep Voltammetry (LSV)

Chronoamperometry (CA)

Chronopotentiometry (CP)

Electrochemical Impedance (EIS)

Featured Research

Al corrosion rates as a function of the applied current with inset SEM micrographs showing representative corrosion morphological evolution. Black diamond symbols depict the corrosion rates determined following Faraday’s law, whereas the pink bars show the experimentally acquired corrosion rates.

Real-time SEM imaging of localized anodic corrosion and hydrogen evolution in aluminum

The Hummingbird Scientific SEM Bulk Liquid Electrochemistry sample holder was used to directly visualize localized anodic corrosion of aluminum at the solid–liquid interface during controlled electrochemical measurements. By combining operando liquid-phase SEM imaging with galvanostatic electrochemical control, researchers monitored the initiation and growth of corrosion pits in real time. The study revealed the progression from early surface blister formation and nanoscale pit nucleation to complex fractal-like dissolution morphologies as corrosion advanced. Operando imaging also captured hydrogen bubble formation at active corrosion fronts, which was subsequently confirmed as molecular hydrogen. The holder’s bulk electrochemistry architecture enabled quantitative electrochemical measurements to be directly connected to dynamic mechanisms governing corrosion initiation and evolution.

Reference: Morgan Barbey-Binggeli, et al. Journal of the American Chemical Society (2025). DOI: 10.1021/jacs.5c11352

Abstract

Video Spotlight

Copper electrodeposition and dissolution visualized in real time within a CuSO₄ electrolyte using the SEM Bulk Liquid Electrochemistry Sample Holder. The corresponding current and voltage profiles show stable, repeatable bulk-representative electrochemical behavior across multiple cycles.

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

Typical in-situ SEM liquid-phase electrochemistry uses on-chip electrodes that can reduce fidelity due to confined geometries, unstable reference potentials, and cycling-induced degradation. The SEM Bulk Liquid Electrochemistry Sample Holder uses off-chip bulk reference and counter electrodes to enable stable, reproducible electrochemical performance that closely reproduces benchtop behavior inside SEM.

The video shows Cu electrodeposition and dissolution in CuSO₄ under alternating potential cycling. Particle morphology evolves with cycle number. Operando SEM reveals Cu cube nucleation in the first cycle, followed by layer growth and partial dissolution, enabling controlled morphology tuning. Cyclic voltammetry remains stable across cycles, confirming bulk-representative electrochemical behavior.

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‍Hummingbird Advantages

Bulk off-chip reference and counter electrodes enable stable, reproducible cycling closely matching benchtop electrochemical behavior.
Operando SEM imaging enables real-time observation of nucleation, growth, and dissolution pathways during electrochemical cycling.

Reference: Philipp Grosse, et al, J. Phys. Chem. C (2020). DOI: 10.1021/acs.jpcc.0c09105

Abstract

High Impact Publications

Trusted by researchers worldwide, the Hummingbird Scientific SEM Bulk Liquid Electrochemistry Sample Holder has been used in multiple peer-reviewed publications demonstrating in-situ electrochemical measurements and correlated structural evolution in liquid environments.

Pit Morphology, Dissolution Kinetics, and Gas Generation Monitored in Real Time during Localized Anodic Aluminum Corrosion

Morgan Barbey-Binggeli, Vasiliki Tileli

Journal of the American Chemical Society

2025

Abstract

In-Situ Liquid-Electrochemical X-Ray and Electron Microscopy for Multi-Modal Energy Materials Characterization

Calvin Parkin, Tyler Mefford, Jongwoo Lim, Aram Yoon, Rui Serra-Maia, Pawan Kumar, See Wee Chee, William C. Chueh, Daan Hein Alsem, Norman Salmon, Eric A. Stach

ECS Meeting Abstracts

2024

Abstract

Graphene Electrode for Studying CO2 Electroreduction Nanocatalysts under Realistic Conditions in Microcells

Saltanat Toleukhanova, Tzu-Hsien Shen, Chen Chang, Swathilakshmi Swathilakshmi, Tecla Bottinelli Montandon, Vasiliki Tileli

Advanced Materials

2024

Abstract

Dynamic Imaging of Nanostructures in an Electrolyte with a Scanning Electron Microscope

Aram Yoon, Antonia Herzog, Philipp Grosse, Daan Hein Alsem, See Wee Chee, Beatriz Roldán Cuenya

Microscopy and Microanalysis

2021

Abstract

Software

Spend less time managing equipment and more time generating results. Hummingbird Connect integrates with microscope and laboratory software platforms to simplify experiment setup, streamline workflows, and keep your data organized from acquisition through analysis.

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To help you get the most from your liquid-cell holder, Hummingbird Control Software provides intuitive and precise control of closed loop liquid heating. Together, these software solutions enable faster setup, improved reproducibility, and more efficient liquid-phase and electrochemical SEM experiments.

Liquid Heating Control

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Hummingbird Connect™Hummingbird Control™ Software

Built on Engineering Excellence

Hummingbird Scientific designs, machines, assembles, tests, and services its products in-house. Our integrated engineering, machining, microfabrication, software development, and applications teams enable rapid product development, custom modifications, and direct technical support throughout the life of the instrument. This vertically integrated approach allows researchers to adapt experimental platforms to unique scientific requirements while maintaining the performance and reliability required for advanced in-situ microscopy experiments.

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The SEM Bulk Liquid Electrochemistry Sample Holder is a direct result of these capabilities, enabling reproducible true bulk electrochemical measurements combined with in-situ nanoscale imaging.

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Need something unique? Our engineers can customize existing products or develop entirely new solutions to support specialized experiments and emerging research challenges.

Engineering Process Custom Solutions

Frequently Asked Questions

Related Products

Awards

Microscopy Today 2021 Innovation Award

Microscopy Today

2021

Hummingbird Scientific was named a 2021 Microscopy Today Innovation Award recipient for its multimodal in situ bulk liquid-electrochemistry microscopy platform.