Energy & Environmental Science
DOE Technical Report
Microscopy and Microanalysis
Nature Communications
The TEM Gas Heating Sample Holder enables in-situ TEM and STEM imaging of dynamic gas–solid reactions under controlled environmental conditions. A sealed environmental cell with electron-transparent silicon nitride (SiN) windows isolates the reactive gas environment from the microscope vacuum 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 imaging during high-temperature experiments. The holder supports compatible microfabricated chips for MEMS heating and electrical biasing, with optional multi-channel gas delivery for controlled gas mixing and advanced in-situ TEM 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, corrosion, thin-film deposition and dissolution, nanoparticle dynamics, temperature-dependent reactions, redox processes, and gas–solid interfacial transformations under controlled gaseous environments.
Gas–solid reactions often involve transient atomic- and nanoscale transformations that determine material performance but are difficult to capture with conventional techniques. By combining controlled gas composition and pressure with closed-loop MEMS heating and electrical biasing, the holder allows correlation of structural evolution with applied stimuli to reveal the reaction pathways and transformations governing material performance, stability, and degradation.

The TEM Gas Heating Sample Holder integrates a sealed environmental cell, all-metal gas delivery tubing, multifunctional microfabricated chips, electrical biasing connections, and dedicated control hardware into a versatile platform for in-situ gas-phase TEM and STEM experiments. The environmental cell is formed by two microfabricated silicon chips with electron-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 vacuum.
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 optional multi-channel delivery supporting controlled mixing of up to eight gases, a dedicated purge line, and real-time output gas analysis. Optimized holder geometry and a low thermal mass MEMS microheater provide stable imaging during high-temperature 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–solid reactions, phase transformations, and degradation processes in real time at atomic resolution.


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

Load gas-cell TEM chips and samples 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 gas-cell assembly, reducing setup complexity while improving experiment-to-experiment reproducibility and imaging reliability.

Perform temperature-controlled gas-phase TEM with homogeneous MEMS heating above 1000 °C, 4-point on-chip temperature sensing, and near-drift-free imaging

Achieve homogeneous heating above 1000 °C during in-situ gas-phase TEM with MEMS microheaters and integrated 4-point on-chip temperature sensing for accurate closed-loop temperature control. Localized heating minimizes thermal load, enabling stable, near-drift-free imaging throughout the operational temperature range for dynamic in-situ gas–solid reaction experiments.

Control gas pressure from high vacuum to 2 bar using one experimental gas and a dedicated purge line for reliable, repeatable gas-phase TEM experiments

The Purgeable 1+1 Channel Gas Delivery System provides precise, software-controlled delivery of one experimental gas over a pressure range from high vacuum (10⁻⁷ Torr) to 2 bar. A dedicated inert-gas purge line enables rapid switching between reaction gases, supporting sequential oxidation, reduction, and other gas–solid reaction studies while minimizing cross-contamination and ensuring reproducible experiments.

Perform correlative gas-phase microscopy across TEM, SEM, and synchrotron X-ray platforms

Our gas heating platform extends beyond TEM with corresponding SEM and X-ray microscopy gas heating holders, enabling seamless correlative characterization across multiple length scales using the same microfabricated chips. By combining complementary imaging and spectroscopy under controlled gas environments, researchers can directly correlate structural, chemical, and functional changes to gain a more complete understanding of gas–solid reactions and material performance.

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

The TEM Gas Heating Sample Holder supports both EDS and EELS, enabling researchers to correlate in-situ gas-phase imaging with real-time chemical and elemental analysis. Optimized environmental cell and microfabricated chip geometries maximize X-ray collection efficiency, while low-bowing membranes and small spacers help reduce gas scattering and maintain sample stability suitable for EELS acquisition.

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

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

Keep experiments moving with in-stock gas-cell TEM chips designed for gas flow, heating, sample biasing, and multimodal microscopy workflows

Hummingbird Scientific manufactures gas-cell TEM chips in our in-house microfabrication and inspection facility and maintains more than 60 standard configurations in stock for rapid delivery. Designed for in-situ TEM gas-flow imaging, biasing, and heating experiments, these chips are ready-to-use out of the box and require no additional cleaning before use. This means your experiments will not get held up by long lead times for substrates. Multiple spacer, window, and heater geometries as well as material options support applications including corrosion studies, phase transformations, and catalysis, with made-to-order custom chips available for specialized experiments.

Unlock superior control of gas composition with on-the-fly mixing of up to eight gases and real-time output gas analysis

The optional Multi-Channel Gas Delivery System provides flexible control over gas composition with up to eight reaction gas inputs and a dedicated vapor line that can be operated independently or simultaneously in user-defined proportions. Gases are mixed within a buffer tank inside the compact control unit, with composition and pressure regulated through the Multi-Channel Gas Delivery Software. The resulting gas mixture is delivered to the environmental cell over a pressure range from high vacuum (10⁻⁷ Torr) to 2 bar. An optional residual gas analyzer (RGA) enables real-time measurement of both inlet and outlet gas composition for comprehensive monitoring of reaction conditions.

HAADF-STEM images of the hybrid supporting oxide a) and the resultant Pt-containing catalysts b–d). e) In-situ tracking of Ce4+ concentration and temperature for the in situ XAS and STXM CO oxidation (1 vol.% CO +4 vol.% O2 + 95 vol.% Ar) experiment. f) Enhanced specific mass activity of PCT during repeated and prolonged CO oxidation reaction. The MA of Pt was increased by 3.3 times from PCT-1 to PCT-10 h. The MA of PT catalyst without Ce addition was increased by 9.6 times upon adding 2 wt.% of Ce (from PT to PCT-1).
In-situ characterization of Pt nanoparticle disintegration during CO oxidation on hybrid oxide supports
The Hummingbird Scientific TEM Gas Heating sample holder was used to directly observe the structural evolution of Pt nanoparticles supported on CeOₓ–TiO₂ hybrid oxides during carbon monoxide oxidation. In-situ STEM imaging under flowing reaction gas conditions revealed the dynamic disintegration of Pt nanoparticles into single atoms and sub-nanometer clusters at elevated temperature, while complementary X-ray spectroscopy and microscopy tracked changes in the support oxidation state. The holder enabled correlation of catalyst morphology with catalytic performance, showing that oxygen-driven restructuring of Pt at the oxide interface led to a threefold increase in mass-specific activity during CO oxidation. These results apply in-situ gas-heating TEM to reveal catalyst activation pathways that are inaccessible through ex-situ characterization.
Reference: Eunji Kang, et al. Small (2025). DOI: 10.1002/smll.202506990
Copyright © 2025 The Author(s). Small publishedby Wiley-VCH GmbH.
Video showing ferrihydrite nanoparticle fragmentation and restructuring during a phase transformation into magnetite in a heated gaseous environment.
In-situ high-temperature ferrihydrite reduction in H₂ gas
Although ferrihydrites do not typically catalyze reactions in gaseous environments, multiple transient Fe-based heterogeneous catalysts such as magnetite can be produced by activation of ferrihydrite nanoparticles via hydrogen reduction, with a strong dependence on applied conditions. The TEM Gas Heating holder enables direct connection of applied pressure, temperature, and beam conditions to transient nanocatalyst formation dynamics.
The video shows ferrihydrite nanoparticle reduction to fragmented magnetite in 1.1 bar of hydrogen gas flown into the TEM gas cell. The imaging stability across the temperature range enabled real-time grain restructuring and phase changes of particles from amorphous to a crystalline structure to be captured as the particle was reduced when heated to 360°C in the presence of H2.
Hummingbird Advantage
Reference: Hummingbird Scientific internal data in collaboration with Jaco Olivier, Matthew Coombes, and Jan Neethling from Nelson Mandela Metropolitan University, South Africa
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 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 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 TEM experiments.
Need something unique? Our engineers can customize existing products or develop entirely new solutions to support specialized experiments and emerging research challenges.
The TEM Gas Heating Sample Holder is an in-situ transmission electron microscopy (TEM) sample holder that uses microfabricated chips to create a sealed environmental cell inside the microscope, maintaining the sample in a controlled gas environment isolated from the microscope vacuum. It enables real-time, atomic-resolution TEM and STEM imaging during gas-phase experiments with controlled gas flow up to 2 bar, closed-loop MEMS heating above 1000 °C, electrical biasing, and optional multi-channel gas delivery of up to eight gases with real-time output gas analysis, allowing researchers to investigate dynamic gas–solid reactions and temperature-dependent material transformations.
The TEM Gas Heating Sample Holder supports a wide range of in-situ gas-phase TEM experiments, including heterogeneous catalysis, oxidation and reduction reactions, corrosion, thin-film deposition and dissolution, nanoparticle dynamics, redox processes, temperature-dependent phase transformations, and gas–solid interfacial studies. Compatible microfabricated chips further enable MEMS heating and electrical biasing, allowing researchers to correlate structural evolution with thermal and electrical stimuli under controlled gas environments in real time.
The TEM Gas Heating Sample Holder supports controlled gas flow over a wide pressure range, from high vacuum to 2 bar, through a standard 1+1 channel gas delivery configuration consisting of one experimental gas line and one dedicated purge gas line. An optional multi-channel gas delivery system enables controlled mixing of up to eight gases, together with real-time output gas analysis, providing precise control of gas composition and pressure for complex reaction environments and advanced in-situ gas-phase TEM and STEM experiments.
The TEM Gas Heating Sample Holder features a precision-engineered, screw-free loading and sealing mechanism that enables fast, reproducible environmental cell assembly. During loading, the mechanism automatically aligns the two silicon nitride (SiN) windows and establishes on-chip electrical connections with the holder, eliminating the requirement for manual window and electrical contact alignment. This streamlined design ensures consistent environmental cell geometry, reduces setup time, minimizes user variability, and delivers reliable, repeatable performance across in-situ gas-phase TEM experiments.
Yes. The TEM Gas Heating Sample Holder supports both EDS and EELS during in-situ gas-phase TEM experiments. Its environmental cell and microfabricated chip design are optimized to maximize X-ray collection efficiency for reliable elemental analysis and mapping while maintaining specimen stability suitable for high-quality EELS measurements. Together, these capabilities allow researchers to correlate real-time structural evolution with elemental composition and chemical information during dynamic gas–solid reactions and high-temperature material transformations.
The TEM Gas Heating Sample Holder is compatible with a wide range of research gases, including 100% hydrogen (H₂), 100% oxygen (O₂), and other non-corrosive research gases commonly used for catalysis, oxidation, reduction, and environmental TEM studies. The all-metal holder body and gas delivery path are resistant to most research gases and can be baked to remove residual trace gases between experiments for clean, repeatable operation. Use of hazardous, toxic, or flammable gases should be coordinated with your microscope facility management and may require dedicated exhaust or outlet gas venting to comply with local laboratory safety requirements.
Yes. The TEM Gas Heating Sample Holder uses compatible microfabricated chips that can be transferred directly between Hummingbird Scientific's TEM, SEM, and X-ray microscopy gas-phase heating platforms. This capability allows researchers to investigate the same sample using complementary microscopy and spectroscopy techniques without changing the sample substrate, simplifying sample transfer and enabling direct correlation of structural, morphological, chemical, and functional information across multiple instruments.
The TEM Gas Heating Sample Holder uses Hummingbird Scientific's in-house microfabricated MEMS chip platform to simplify experiment planning while providing exceptional flexibility for in-situ gas-phase TEM. Standard heating, electrical biasing, and specialized gas-environment MEMS chips are quality controlled, in stock, and ready to ship within 24 hours through Hummingbird Scientific's online store. A broad selection of heater configurations, electrode materials, electrode layouts, and silicon nitride (SiN) window geometries allows researchers to optimize chips for a wide range of gas-phase experiments. Clean-packed chips are ready to use out of the box, while the same MEMS chip platform is compatible across Hummingbird Scientific's TEM, SEM, and synchrotron X-ray heating and biasing systems. For specialized applications, Hummingbird Scientific also develops custom MEMS chip designs tailored to unique devices, reaction environments, and experimental workflows.

