The X-ray Gas Heating Sample Holder enables in-situ X-ray microscopy and spectroscopy of dynamic gas–solid reactions under controlled environmental conditions. A sealed environmental cell with X-ray transparent silicon nitride (SiN) windows isolates the reactive gas environment from the microscope environment while supporting gas flow up to 2 bar and closed-loop MEMS heating above 1000 °C. A precision-engineered, screw-free loading and sealing mechanism enables fast, reproducible sample loading and automatic window alignment. Optimized holder geometry and a low thermal mass MEMS microheater provide stable sample positioning during high-temperature operando experiments. The platform supports compatible microfabricated chips for MEMS heating and electrical biasing, with optional multi-channel gas delivery for controlled gas mixing and advanced in-situ X-ray studies.
Designed for researchers in materials science, chemistry, catalysis, energy storage, environmental science, and nanotechnology, the platform enables in-situ investigation of heterogeneous catalyst performance, oxidation and corrosion, thin-film growth and degradation, nanoparticle evolution, temperature-dependent reactions, redox processes, and gas–solid interfacial transformations under controlled gaseous environments using X-ray microscopy and spectroscopy.
Gas–solid reactions often involve dynamic structural and chemical transformations that determine material performance but are difficult to capture with conventional techniques. 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 combining controlled gas composition and pressure with closed-loop MEMS heating and optional electrical biasing, the holder allows correlation of structural evolution, chemical changes, and applied stimuli to reveal the reaction pathways and mechanisms governing material performance, stability, and degradation.
The X-ray Gas Heating Sample Holder integrates a sealed environmental cell, metal & PEEKsil gas delivery tubing, multifunctional microfabricated chips, electrical biasing connections, and dedicated control hardware into a versatile platform for in-situ gas-phase X-ray microscopy and spectroscopy. The environmental cell is formed by two microfabricated silicon chips with X-ray transparent silicon nitride (SiN) windows. A sample is loaded onto one of the chips before the two chips are sealed together, creating a controlled gas environment around the specimen that remains isolated from the microscope environment.
A precision-engineered, screw-free loading and sealing mechanism enables fast, reproducible sample loading and automatic alignment of the SiN windows. Controlled gas flow is delivered through the sealed environmental cell at pressures up to 2 bar using Hummingbird Scientific's gas delivery systems, with a dedicated purge line for rapid contamination-free experimental gas switching. Optimized holder geometry and a low thermal mass MEMS microheater provide stable sample positioning during in-situ experiments with closed-loop heating above 1000 °C and integrated 4-point on-chip temperature sensing.
Compatible microfabricated chips for MEMS heating and electrical biasing enable thermal and electrical stimuli to be applied during controlled gas-phase experiments, allowing researchers to observe gas-induced structural transformations, chemical evolution, catalyst activation, oxidation, phase transformations, and degradation processes in real time under realistic reaction environments.
Achieve reproducible gas-cell assembly with self-aligning windows and a screw-free sealing design
Perform temperature-controlled gas-phase X-ray microscopy and spectroscopy with homogeneous MEMS heating above 1000 °C, 4-point on-chip temperature sensing, and near-drift-free performance
Control gas pressure from high vacuum to 2 bar using one experimental gas and a dedicated purge line for reliable, repeatable gas-phase X-ray microscopy and spectroscopy experiments
Configure the holder for seamless integration with synchrotron beamlines and laboratory X-ray microscopy systems
Perform correlative gas-phase microscopy across TEM, SEM, and synchrotron X-ray platforms
Protect your X-ray microscope's vacuum chamber during gas-cell experiments and streamline experimental workflows with rapid high-vacuum seal checking
Keep experiments moving with in-stock gas-cell X-ray chips designed for gas flow, heating, sample biasing, and multimodal microscopy workflows
a) Schematic illustration of the setup showing the gas-flow cell. b) Schematic of the electron beam and X-ray directions for SFXM and TEM imaging on particle I,a truncated cube. c) TEM overview of Cu2O particles inside the nanoreactor. The red circle indicates particle I. d) TEM image showing particle I with the electron beam parallel to the direction of the Cu2O cube. e) Low-resolution SFXM image of the particles using Cu Kα and Ni Kα emission with a white circle indicating particle I. f) High-resolution SFXM image of particle I from Cu Kα emission.
Operando X-ray microscopy of facet-dependent Cu₂O photocatalysis during CO₂ reduction
The Hummingbird Scientific X-ray Gas Heating sample holder enabled correlative operando X-ray microscopy and environmental TEM measurements of individual Cu2O photocatalyst particles under realistic CO2/H2O reaction conditions. Using a gas-flow nanoreactor with optical illumination, researchers directly monitored chemical-state changes and structural dynamics on specific crystal facets during photocatalytic CO2 reduction. The platform revealed that Cu2O (110) facets actively adsorb and reduce CO2 to methanol, while (100) facets remain largely inactive. Combined X-ray spectroscopy, EELS, and diffraction measurements showed reversible Cu(I)/Cu(II) redox cycling and lattice expansion during CO2 adsorption, providing direct insight into the active sites responsible for highly selective solar-driven methanol production.
Reference: Yimin A. Wu, et al. Nature Energy (2019). DOI: 10.1038/s41560-019-0490-3
Copyright © 2019, This is a U.S. government work and not under copyright protection in the U.S.; foreign copyright protection may apply
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 gas-cell holder, Hummingbird Control Software provides intuitive and precise control of closed loop gas heating. Together, these software solutions enable faster setup, improved reproducibility, and more efficient gas-phase SEM 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 X-ray Gas Heating Sample Holder is a direct result of these capabilities, integrating controlled gas delivery, MEMS heating, and experimental workflows into a single platform for reproducible in-situ gas-phase X-ray experiments.
Need something unique? Our engineers can customize existing products or develop entirely new solutions to support specialized experiments and emerging research challenges.
