ECS Meeting Abstracts
Microscopy and Microanalysis
Joule
ECS Meeting Abstracts
The Hummingbird Scientific X-ray Bulk Liquid Electrochemistry Sample Holder enables in-situ synchrotron X-ray microscopy and spectroscopy with true bulk liquid electrochemistry. A sealed liquid cell combined with off-chip bulk reference (e.g., Ag/AgCl) and counter (e.g., Pt) electrodes delivers stable, reproducible electrochemical measurements that closely replicate conventional benchtop three-electrode experiments while enabling real-time correlation of structural, chemical, and electrochemical changes.
Ideal for researchers studying liquid-phase electrochemical processes in batteries, electrocatalysts, and energy materials, where direct observation of reaction mechanisms, material structure, and chemical evolution at the nanoscale is critical.
Electrochemical measurements alone often cannot reveal why materials succeed, degrade, or fail. The holder is optimized for versatilty in a wide array of high-resolution X-ray synchrotron beamline endstation configurations wherein multiple unique detectors including scattered and transmission are oriented around the sample stage inside of a high-vacuum chamber. By directly correlating electrochemical data with real-time nanoscale chemical 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 X-ray 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 X-ray microscope. 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 X-ray illumination. 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 in-situ liquid-cell systems that rely on on-chip pseudo-reference electrodes, the X-ray 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.

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

Load liquid-cell X-ray 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.

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 X-ray Bulk Liquid Electrochemistry Sample Holder features a removable tip, allowing access for tubing replacement, and capability upgrades.

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

Perform in-situ liquid-phase X-ray microscopy 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.

Configure the holder for seamless integration with synchrotron beamlines and laboratory X-ray microscopy systems

Hummingbird Scientific works directly with researchers to configure the X-ray Bulk Liquid Electrochemistry Sample Holder for specific synchrotron beamlines and laboratory X-ray microscopy platforms. Engineering integration can include microscope interface development, liquid cell configuration, bulk electrode configuration, MEMS chip configuration, and sample holder modifications for application-specific functionality. This collaborative approach enables researchers to implement in-situ bulk liquid electrochemistry while maintaining compatibility with existing X-ray instrumentation and evolving experimental requirements.

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

Our bulk liquid electrochemistry platform extends beyond the X-ray synchrotron beamline with compatible holders for TEM and SEM 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.

Protect your X-ray microscope's vacuum chamber during liquid-cell experiments and streamline experimental workflows with rapid high-vacuum seal checking

Reliable in-situ liquid flow 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 performance.

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

Hummingbird Scientific manufactures liquid-cell X-ray microscopy chips in our in-house microfabrication facility and maintains more than 60 standard configurations in stock for rapid delivery. Designed for in-situ X-ray microscopy liquid-flow imaging, electrochemistry, and heating experiments, these chips are ready-to-use out of the box and require no additional cleaning. This means your experiments will not get held up by long lead times for substrates. Multiple spacer, window, heater, 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 X-ray microscopy capabilities with homogeneous heating concurrent with electrochemical control, precise temperature regulation, and near-drift-free in-situ imaging

The Integrated Liquid Heating system enables controlled thermal stimulation alongside simultaneous electrode biasing control, directly within the liquid cell for temperature-dependent in-situ electrochemistry 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 X-ray microscopy, capturing dynamic liquid-liquid 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 X-ray Bulk Liquid Electrochemistry sample holder with the BioLogic SP-200 potentiostat for quantitative in-situ X-ray electrochemistry

The BioLogic SP-200 Potentiostat extends the capabilities of the X-ray Bulk Liquid Electrochemistry Sample Holder by enabling quantitative electrochemical measurements during in-situ X-ray microscopy and spectroscopy. 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.

a) Schematic of Li/Li+ cycling in LiNi1/3Mn1/3Co1/3O2 particles under operando liquid-electrochemical STXM. b) Quantified heterogeneity for various charging C-rates and imaging conditions. c) Li concentration for two charge/discharge rates showing heterogeneity differences measured in (b).
Operando X-ray spectromicroscopy of strain-driven lithium transport in single-crystal NMC cathode particles
The Hummingbird Scientific X-ray Bulk Liquid Electrochemistry sample holder enabled operando electrochemical cycling and high-resolution X-ray spectromicroscopy of single-crystalline LiNi1/3Mn1/3Co1/3O2(scNMC) battery cathode particles. Operando scanning transmission X-ray microscopy (STXM) was combined with post-cycling Bragg coherent diffraction X-ray imaging to correlate lithium distribution with three-dimensional strain fields during charge and discharge. Using the holder’s bulk off-chip counter and reference electrodes, researchers observed unexpected fluctuation of lithium-rich and lithium-poor regions within individual particles, revealing that nanoscale lithium transport can proceed counter to concentration gradients. The study demonstrated how strain influences lithium diffusion and revealed that controlling lithium distribution near particle surfaces may improve battery rate performance.
Reference: Danwon Lee, et al. Nature Communications (2025). DOI:10.1038/s41467-025-64068-9
Copyright © 2025 The Author(s). Nature Communications published by Springer Nature. Open Access.
X-ray chemical maps of LiFePO₄ nanoparticles during charging and discharging. Experimental STXM results and simulated results show strong agreement. Scale bar: 1 μm.
STXM investigation of Li battery particle charging and discharging
Because rechargeable battery degradation is in part due to physical changes in the electrodes caused by electrochemical cycling, optimization of the kinetics and uniformity of ion insertion can extend Li-ion battery lifetimes. The X-ray Generation V Bulk Liquid Electrochemistry sample holder enables reproducible connection of applied charging conditions, electrolyte chemistry, and battery particle morphology to lithiation and delithiation dynamics.
The video shows scanning transmission X-ray microscopy (STXM) sequences of delithation (charging) and lithiation (discharging) processes for several Li-ion battery particles, tracking Fe oxidation states and mapping to Li+ concentration via the exchange current density. Composition dependence of the Li+ insertion rate constant amplifies nonuniformities during delithiation but suppresses them during lithiation, stabilizing the solid solution.
Hummingbird Advantages
Reference: Jongwoo Lim, et al, Science (2016). DOI: 10.1126/science.aaf4914
Video Copyright © 2016, American Association for the Advancement of Science
Hummingbird Control™ supports liquid heating workflows when the holder is configured with the liquid-heating controller. The software enables temperature setpoint control, real-time monitoring, closed-loop or open-loop operation, and exportable temperature data for supported liquid-phase experiments.
Hummingbird Connect™ supports experiment organization by connecting holder setup, microscope context, imaging conditions, and experiment metadata for repeatable in situ X-ray electrochemistry workflows.
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 X-ray Bulk Liquid Electrochemistry Sample Holder is a direct result of these capabilities, enabling reproducible true bulk electrochemical measurements combined with in-situ X-ray spectroscopy and microscopy.
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 X-ray 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 vacuum chamber of a high-resolution synchrotron beamline. 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 imagingor spectroscopy 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.
Unlike fully on-chip three-electrode systems, the X-ray 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.
Hummingbird Control™ provides intuitive control and monitoring of experiment parameters such as temperature, biasing voltage, current, etc. during in-situ SEM 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.
The Hummingbird Scientific X-ray Bulk Liquid Electrochemistry Sample Holder enables a broad range of in-situ X-ray 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.
The X-ray 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.
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.
The X-ray Bulk Liquid Electrochemistry Sample Holder is custom integrated for compatibility with virtually all synchrotron X-ray microscopy end stations. Final compatibility is determined by the specific microscope configuration, beamline geometry, holder interface, sample environment, and experimental requirements, ensuring an optimized solution for each instrument and application. Our standard design is optimized for high-resolution synchrotron XAS, STXM, and X-ray ptychography beamlines, where the enclosed liquid cell must be mounted in a vacuum chamber.
Yes. Hummingbird Scientific can support custom integration and workflow-specific modifications involving holder interfaces, sample chips, electrode configurations, spacer/window requirements, heating control, and beamline or laboratory X-ray microscope constraints.



