Perform in-situ synchrotron X-ray microscopy with bulk liquid electrochemistry using off-chip reference and counter electrodes for stable, reproducible measurements.

True Bulk Liquid Electrochemistry for in-situ Synchrotron X-ray Microscopes

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.

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, material structure, and chemical evolution at the nanoscale is critical.

Understand What Drives Electrochemical Performance

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.

X-Ray Bulk Liquid Electrochemistry Sample Holder

Hummingbird Advantages:

  • Replicates benchtop electrochemical measurements inside the X-ray microscope or beamline
  • 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 and spectroscopy of material transformations and degradation mechanisms
  • Features screw-free liquid-cell assembly with self-aligning windows for fast, reproducible sample loading
  • Compatible with X-ray microscopy, TEM, and SEM workflows using cross-platform microfabricated chips
Technical Specs
1470 Series X-Ray
Total Electrodes
6
Reference Electrode
Yes
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 Compatibility
Yes
Beamline Compatibility
Custom integration possible for all endstation chambers, optimized for high-resolution XAS, STXM, and ptychography beamlines where high vacuum chambers are required

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 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.

Key Features and Capabilities

True Bulk Electrochemistry

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

Reproducible Screw-Free Liquid-Cell Assembly

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

Removable, Swappable Tip and Tubing

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

Flexible Liquid Cell Operation

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

Custom X-ray Microscope Integration

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

Multimodal Imaging

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

X-ray Safety & Seal Verification

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

60+ In-Stock Liquid-Cell X-ray Microscopy Chip Configurations

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

Optional add-on feature
Integrated Liquid Heating

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

Optional add-on feature
Dual-Flow Liquid Mixing

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 add-on feature
Biologic SP-200 Potentiostat

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

Featured Research

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.

Video Spotlight

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

  • Bulk reference and counter electrodes allow direct extrapolation of observed lithiation/delithiation mechanisms to bulk battery design and chemistry.
  • Robust off-chip electrodes minimize electrode degradation over many electrochemical cycles.

Reference: Jongwoo Lim, et al, Science (2016). DOI: 10.1126/science.aaf4914

Video Copyright © 2016, American Association for the Advancement of Science

High Impact Publications

Trusted by researchers worldwide, the Hummingbird Scientific X-ray Bulk Liquid Electrochemistry Sample Holder has supported peer-reviewed research demonstrating in-situ electrochemical measurements and correlated structural and chemical evolution under realistic bulk liquid conditions.

(Battery Student Slam 8 Award Winner) Multi-Clustered Lithium Diffusion in Single-Crystalline NMC Battery Particles

Danwon Lee, Chihyun Nam, Juwon Kim, Bonho Koo, Hyejeong Hyun, Jinkyu Chung, Sungjae Seo, Munsoo Song, Jaejung Song, Daan Alsem, Norman Salmon, Suyong Lee, Namdong Kim, David Shapiro, Jongwoo Lim

ECS Meeting Abstracts

2024
Tracking Morphology and Chemical State of Electrocatalysts during Reaction through Correlated Electron Microscopy, X-ray Microscopy and X-ray Absorption Spectroscopy Experiments

See Wee Chee, Aram Yoon, Shih-Yu Fu, Beatriz Roldan Cuenya

Microscopy and Microanalysis

2024
Spatiotemporal active phase evolution for CO2 electrocatalysis

Juwon Kim, Si Young Lee, Se-Jun Kim, Bonho Koo, Jinkyu Chung, Danwon Lee, Subin Choi, Jimin Kim, Sungjae Seo, Chihyun Nam, Karl Adrian Gandionco, Gwangsu Bak, Sugeun Jo, Namdong Kim, Hyun-Joon Shin, Keun Hwa Chae, Da Hye Won, Matthew A. Marcus, David A. Shapiro, Shu-Chih Haw, Daan Hein Alsem, Norman J. Salmon, Byoung Koun Min, Hyungjun Kim, Yun Jeong Hwang, Jongwoo Lim

Joule

2024
Nanoscopic Strain-Associated Lithium Diffusion in Single-Crystalline NMC Battery Particles

Danwon Lee, Chihyun Nam, Juwon Kim, Bonho Koo, Hyejeong Hyun, Jinkyu Chung, Sungjae Seo, Munsoo Song, Jaejung Song, Daan Hein Alsem, Norman Salmon, Suyong Lee, Namdong Kim, David Shapiro, Jongwoo Lim

ECS Meeting Abstracts

2024

Software

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.

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 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.

Frequently Asked Questions

What is an X-Ray Bulk Liquid Electrochemistry Sample Holder?
How does in-situ X-ray bulk electrochemistry compare with benchtop electrochemistry?
What does software do in an in-situ microscopy experiment?
What types of experiments can be performed with the X-ray Bulk Liquid Electrochemistry Sample Holder?
Which reference and counter electrode materials are supported by the X-ray Bulk Liquid Electrochemistry Sample Holder?
How is the liquid flow controlled in the X-ray Bulk Liquid Electrochemistry Sample Holder?
Is the X-ray Bulk Liquid Electrochemistry Sample Holder compatible with my X-ray microscope or beamline?
Can the X-ray Bulk Electrochemistry Sample Holder be customized for specialized X-ray workflows?

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.

Macres Award

Microanalysis Society
2018
Daan Hein Alsem received the 2018 Macres Award for Best Instrumentation/Software Paper for X-ray liquid electrochemistry work with the Prof. Chueh group.
X-ray Bulk Liquid Electrochemistry
Technical Specs
1470 Series X-Ray
Total Electrodes
6
Reference Electrode
Yes
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 Compatibility
Yes
Beamline Compatibility
Custom integration possible for all endstation chambers, optimized for high-resolution XAS, STXM, and ptychography beamlines where high vacuum chambers are required
Instrument Type
X-ray
Full Product Information
Product Specifications
Fill out the following form to receive a quote
Biologic SP-200 Potentiostat
Integrated Liquid Heating
Dual-Flow Liquid Mixing