Microscopy and Microanalysis
ECS Meeting Abstracts
Microscopy and Microanalysis
Journal of the American Chemical Society
The Hummingbird Scientific TEM Bulk Liquid Electrochemistry Sample Holder is the first in-situ liquid-phase TEM platform designed to reproduce true bulk electrochemical behavior inside the TEM. Unlike conventional liquid-cell TEM systems that use 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.
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.
Electrochemical measurements alone often cannot reveal why materials degrade, fail, or outperform other materials. 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.

The TEM 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 TEM. 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.
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.


Perform in-situ liquid-phase electrochemistry that matches benchtop performance

Unlike conventional liquid-cell TEM systems that rely on on-chip pseudo-reference electrodes, the TEM bulk liquid electrochemistry sample holder incorporates bulk off-chip reference and counter electrodes. This architecture delivers stable reference potentials, reduced signal drift, and electrochemical measurements that closely match benchtop experiments as shown in the image on the left.

Achieve reproducible liquid-cell assembly with self-aligning windows and a screw-free sealing design

Load liquid-cell TEM chips and solutions in minutes using our industry-leading ease-of-use constant-compression tip sealing mechanism. The tight-tolerance chips fit perfectly into the precision-machined tip, repeatably self-aligning the SiN viewing membranes and evenly compressing the O-rings without relying on finicky screws or alignment jigs. The precision-machined holder tip delivers consistent liquid-cell assembly, reducing setup complexity while improving experiment-to-experiment reproducibility and imaging reliability.

Image samples in continuous-flow or static liquid environments using a sealed microfluidic chip assembly

Perform in-situ liquid-phase TEM experiments under flowing or static liquid conditions while maintaining microscope safety, experimental flexibility, and reproducible imaging. The sealed microfluidic liquid-cell architecture supports a wide range of electrochemistry, catalysis, synthesis, and materials characterization applications.

Simplify cleaning with removable and upgradeable holder tips that allow user access for full tubing replacement

Clean up after your experiment with ease so you can avoid cross-contamination. The Hummingbird Scientific TEM Bulk Liquid Electrochemistry Sample Holder features a removable tip, allowing access for tubing replacement, cell orientation flipping to optimize for TEM or STEM imaging, and capability upgrades.

Correlate electrochemical and imaging data across TEM, SEM, and X-ray microscopy platforms

Our bulk liquid electrochemistry platform extends beyond TEM with compatible holders for SEM and X-ray microscopy platforms, enabling seamless correlative in-situ characterization across multiple length scales using the same electrochemistry chips. This integrated workflow combines real-time electroanalytical measurements with complementary imaging and spectroscopy, providing a more complete understanding of dynamic material behavior under realistic operating conditions.

Perform correlative spectroscopy and microscopy for detailed in-situ elemental analysis

The TEM Bulk Liquid Electrochemistry Sample Holder supports both EDS and EELS, enabling researchers to correlate electrochemical performance with real-time chemical and structural changes. Optimized liquid-cell geometries maximize X-ray collection efficiency while low-bowing membranes and small spacers help reduce liquid scattering and maintain sample stability suitable for EELS acquisition.

Protect your TEM during liquid-cell experiments and streamline setup with rapid high-vacuum seal checking and optical inspection

Reliable in-situ liquid electrochemistry experiments begin well before the holder enters the microscope. Hummingbird Scientific's integrated pumping and seal-checking system helps researchers verify liquid-cell integrity, reduce contamination risk, and protect microscope vacuum performance.

Keep experiments moving with in-stock liquid-cell TEM chips designed for electrochemistry, liquid flow, heating, and multimodal microscopy workflows

Hummingbird Scientific manufactures liquid-cell TEM chips in-house and maintains more than 60 standard configurations in stock for rapid delivery. Designed for in-situ TEM liquid-flow imaging, electrochemistry, and heating experiments, these chips are ready-to-use out of the box and require no additional cleaning. Multiple spacer, window, and electrode geometries as well as material options support applications including corrosion studies, battery research, and electrocatalysis, with made-to-order custom chips available for specialized experiments.

Add temperature-controlled liquid-phase TEM capabilities with homogeneous heating, precise temperature regulation, and near-drift-free in-situ imaging

The Integrated Liquid Heating system enables controlled thermal stimulation directly within the liquid cell for temperature-dependent in-situ TEM experiments. Microfabricated heating chips with calibrated sensors and closed-loop temperature control provide accurate, homogeneous heating up to the boiling point of your solution while maintaining stable imaging conditions.

Accelerate discovery with dual-flow liquid mixing for in-situ liquid phase TEM, capturing dynamic reactions with greater control and flexibility

Optional dual-flow mixing configuration introduces two independent liquid streams into a single liquid-cell, enabling researchers to trigger reactions immediately before observation and capture transient processes as they occur.

Expand the capabilities of the TEM Bulk Liquid Electrochemistry Sample Holder with the BioLogic SP-200 potentiostat for quantitative in-situ TEM electrochemistry

The BioLogic SP-200 Potentiostat extends the capabilities of the TEM Bulk Liquid Electrochemistry Sample Holder by enabling quantitative electrochemical measurements during in-situ TEM and STEM imaging. Combined with Hummingbird Scientific's off-chip bulk reference and counter electrodes, the system replicates conventional benchtop electrochemical measurements while simultaneously capturing nanoscale structural evolution. It supports a wide range of electrochemical techniques, including cyclic voltammetry, chronoamperometry, chronopotentiometry, and battery charge–discharge studies, allowing direct correlation of electrochemical performance with real-time imaging.

In-situ correlative liquid TEM and transmission X-ray microscopy (TXM). a) correlative in-situ TEM and b) TXM showing structure and valence state (bottom). c) Schematic of restructuring mechanisms of Cu2O under NO3RR. d) Yield rate of NO2− and NH3 in the reaction.
Operando liquid-cell TEM imaging of Cu₂O nanocube restructuring during nitrate electroreduction
The Hummingbird Scientific TEM Bulk Liquid Electrochemistry Sample Holder was used to directly visualize the structural evolution of Cu2O nanocube electrocatalysts during the nitrate reduction reaction (NO3RR). Using liquid-cell electrochemical TEM with bulk off-chip reference and counter electrodes, researchers tracked catalyst restructuring in real time under applied electrochemical bias while maintaining quantitatively accurate electrochemical measurements. The operando TEM experiments revealed that Cu2O nanocubes evolve into distinct catalyst morphologies depending on applied potential and electrolyte composition. Under moderately reducing conditions, Cu2O remained stabilized alongside metallic copper due to surface hydroxide formation, correlating with enhanced ammonia selectivity. The study demonstrated how operando TEM can directly connect catalyst restructuring mechanisms to electrochemical performance under typical applied conditions.
Reference: Aram Yoon, et al. Nature Materials (2025). DOI:10.1038/s41563-024-02084-8
Copyright © 2025 TheAuthor(s). Published by Springer Nature Limited. Licensed under the Creative Commons Attribution 4.0 International License (CC BY 4.0).
Copper electrodeposition and dissolution visualized in real time within a CuSO₄ electrolyte using the TEM Bulk Liquid Electrochemistry Sample Holder. The corresponding cyclic voltammetry (CV) data (inset) shows reproducible, bulk-representative electrochemical behavior.
Operando cyclic voltammetry of Cu plating and stripping reproduces benchtop CV over many cycles
Typical in-situ liquid-phase TEM electrochemistry relies on thin film on-chip electrodes, which limits electrochemical fidelity due to constrained geometries, unstable pseudo-reference potentials, and electrode degradation over repeated cycling. The TEM bulk liquid electrochemistry sample holder overcomes these challenges by incorporating bulk, off-chip reference and counter electrodes, enabling reproducible, benchtop-equivalent electrochemical performance inside the TEM.
The video shows copper plating and stripping from a CuSO₄ solution at the working electrode, directly visualized in real time. The corresponding cyclic voltammetry curve (inset) aligns with the observed dynamics, demonstrating consistent and repeatable bulk-representative electrochemical behavior within the in-situ liquid cell TEM experiment.
Hummingbird Advantages
Reference: HBS internal data obtained in collaboration with Rui Filipe Serra Maia and Eric Stach at the University of Pennsylvania.
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.
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 TEM experiments.
Hummingbird Scientific designs, machines, assembles, tests, and services its products in-house. Our integrated engineering, machining, microfabrication, software development, and applications teams enable rapid prototyping and iteration, 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.
The TEM Bulk Liquid Electrochemistry Sample Holder is a direct result of these capabilities, enabling reproducible true bulk electrochemical measurements combined with in-situ nanoscale imaging.
Need something unique? Our engineers can customize existing products or develop entirely new solutions to support specialized experiments and emerging research challenges.
A bulk electrochemistry TEM sample holder is an in-situ transmission electron microscopy sample holder platform that incorporates off-chip reference and counter electrodes, usually Ag/AgCl and Pt, to reproduce bulk electrochemical behavior during real-time in-situ electrochemical experiments in an enclosed liquid cell inside the TEM. The microfabricated chip pair forms a microfluidic channel across the SiN viewing membrane with a patterned working electrode. Liquid is driven through the channel from an external reservoir and imaging is performed through the enclosed liquid layer while the on-chip working electrode and bulk counter and reference electrodes make up a three electrode system for electrochemistry.
Conventional liquid cell TEM systems are limited to on-chip electrode configurations that have constrained geometry and limited electrode material options. These often experience parasitic currents and electrode degradation after repeated cycling, resulting in non-repeatable electrochemical results. The bulk electrochemistry TEM sample holder incorporates dedicated off-chip bulk reference and counter electrodes, providing stable reference potential and current flow for accurate and reproducible electroanalytical performance. Read more in the comparison table above.
Unlike fully on-chip three-electrode systems, the TEM Bulk Liquid Electrochemistry Sample Holder closely matches the performance and repeatability of conventional benchtop electrochemistry by using off-chip reference and counter electrodes. Across multiple electrochemical systems, including copper deposition/stripping and iron redox CV experiments, it produces stable, well-defined redox peaks that remain consistent over repeated cycles and closely match bulk electrochemical behavior.
The Hummingbird Scientific TEM Bulk Liquid Electrochemistry Sample Holder enables a broad range of in-situ TEM electrochemistry experiments. Supported techniques include cyclic voltammetry, chronoamperometry, chronopotentiometry, and controlled battery charge-discharge studies. Researchers can investigate battery materials, electrocatalysts, corrosion, electroplating, electrodeposition, energy conversion, and energy storage while directly correlating electrochemical response with nanoscale structural evolution, phase transformations, and degradation mechanisms in real time.
Hummingbird Control™ provides intuitive control and monitoring of experiment parameters such as temperature, biasing voltage, current, etc. during in-situ TEM electrochemistry experiments. Researchers can configure operating parameters, run controlled experimental profiles, monitor system behavior in real time, and record time-resolved data for accurate analysis and reproducible workflows.
For advanced electrochemical techniques such as cyclic voltammetry, chronoamperometry, and high-sensitivity current measurements, dedicated potentiostat software—such as EC-Lab® for BioLogic® potentiostats—is used to control the electrochemical experiment and acquire measurement data.
Hummingbird Connect™ complements these workflows by consolidating holder parameters, microscope settings and metadata, TEM images and movies, and measurement data from third-party software into a single, unified platform. This integrated workflow helps researchers organize experiments, correlate imaging with experimental conditions, improve reproducibility, and maintain comprehensive records of in-situ TEM electrochemistry studies.
The TEM Bulk Liquid Electrochemistry Sample Holder is designed to support a wide range of standard bulk electrochemical reference and counter electrodes. Common reference electrodes include Ag/AgCl and other custom reference electrode configurations, while counter electrodes can be fabricated from materials such as platinum, gold, graphite, or other chemically compatible conductors. Because the holder uses off-chip bulk electrodes rather than integrated on-chip pseudo-reference electrodes, researchers can select electrode materials that best match their electrolyte chemistry and experimental requirements, enabling more accurate and reproducible in-situ electrochemical measurements.
Yes. The TEM Bulk Liquid Electrochemistry Sample Holder supports both EDS and EELS during in-situ experiments. Its EDS-optimized liquid cell design maximizes X-ray collection efficiency for reliable elemental analysis and mapping. There will always be increased background signature in the EELS signal due to the liquid layer, but the combination of our thinnest microfludic liquid spacers and extreme sample stability enables high-quality EELS measurements to be acquired. Together, these capabilities allow researchers to correlate real-time structural changes with compositional and chemical information during dynamic electrochemical processes.
We supply a microfluidic liquid delivery system with the sample holder, either flow rate or pressure-controlled systems are available. Delivery system operation is covered in the liquid holder training.


