In Situ TEM Gas & Heating
Climate Application Fields
Catalysis
Nanomaterial Growth
Corrosion
Climate Application Fields
Catalysis
Nanomaterial Growth
Corrosion
Observe & Control chemical reactions at the nano-scale
The Climate In Situ TEM Gas & Heating System enables atomic resolution imaging of gas-solid interactions and sample dynamics in research areas such as catalysis, nanomaterials growth and corrosion studies. The Nano-Reactor is the ‘lab on chip’ MEMS based technology enabling up to 2 Bar pressure & elevated temperature environment for in situ TEM. The Climate system converts high-vacuum (S)TEMs from a static imaging tool into a dynamic in situ chemical laboratory, enabling real-time observation and analysis of materials!
Observe & Control chemical reactions at the nano-scale
The Climate In Situ TEM Gas & Heating System enables atomic resolution imaging of gas-solid interactions and sample dynamics in research areas such as catalysis, nanomaterials growth and corrosion studies.
The Nano-Reactor is the ‘lab on chip’ MEMS based technology enabling the 1 Bar pressure & elevated temperature environment for in situ TEM. The Climate system converts high-vacuum (S)TEMs from a static imaging tool into a dynamic in situ chemical laboratory, enabling real-time observation and analysis of materials!
The 8 in 1 solution
The Climate system brings an ‘integrated’ approach to TEM characterisation of catalysts. Previously only possible with a number of separate techniques, Climate in conjunction with the TEM combines the following 8 separate techniques into one seamless platform.
- 1) Size
- 2) Shape
- 3) Crystal structure
- 4) Atomic Structure
- 5) Chemical Bonding
- 6) Calorimetry
- 7) Gas Analysis
- 8) Chemistry
Real-time imaging of catalyst activityExperiment: Ni exposed to 500 mBar He:H2:O2 at 730 °C In this in situ TEM video using the Climate system, a heterogeneous catalyst, Ni oxide, was first reduced before a gas flow of Helium + Hydrogen + Oxygen was introduced to the Nano-Reactor at 730 °C. This video clearly shows certain regions of active particles and others that are inactive. This highlights which catalyst particles really contribute to the reaction, thus, enabling a way to investigate, understand and improve the activity on the single particle level. Interestingly, seen in the top right of this video, one particle shows very unusual shape dynamics for a metal catalyst and provides insight into catalytic reaction mechanics and performance. Click the next tab to view the shape dynamics of this particle at higher resolution. |
Metal catalyst dynamics revealed by In Situ TEMExperiment: Ni exposed to 500 mBar He:H2:O2 at 730 °C This in situ TEM video clearly visualises the structure dynamics of the Ni catalyst particle oscillating through three stages of the catalytic reaction process – (1) activation, (2) the working state under reaction conditions and (3) recovery from the working state to its initial state. The drastic morphological change suggests that the cycle variation may not only be limited to the surface structure, however, takes place throughout the entire particle. Although little modelling has been identified which support such dynamics in metal catalysts, it highlights that using in situ TEM techniques for catalyst research can reveal unexpected and exciting scientific phenomenon. |
Single particle electron diffractionExperiment: Ni exposed to 500 mBar He:H2:O2 at 730 °C The investigation and understanding of catalyst mechanics requires observation of the crystal structure evolution. Commonly, the in situ X-Ray Diffraction based on a synchrotron source is used for obtaining such information, however, averages the information over a large amount of particles. In situ TEM selected area electron diffraction (SAED) opens a door to closely investigate the dynamic crystalline evolution of a single particle and can be carried out on every TEM. Experiment data from Dr. Marc Willinger & Dr. Ramzi Farra, Fritz-Haber-Institute fur der Max-Planck-Gesellschaft, Germany. |
Atomic resolution surface dynamicsExperiment: Cu exposed to 500 mBar H2:N2:O2 at 350 °C This in situ movie was recorded showing the real-time structure dynamics of Cu nanoparticles in a reaction environment at atomic resolution. The images indicate that the surface with a certain orientation shows oscillatory behaviour while other surfaces are not active. With this knowledge, the design and synthesis of catalysts can be optimised to achieve higher reactive productivity. Experiment data from Dr. Marc Willinger & Dr. Ramzi Farra, Fritz-Haber-Institute fur der Max-Planck-Gesellschaft, Germany & Dr. Qiang Xu, DENSsolutions, The Netherlands. |
Measuring chemical bonding evolution using EELSExperiment: CuO exposed to 500 mBar H2:N2:O2 at 350 °C The chemical bonding evolution of catalysts in the real-working environment is challenging to obtain. Commonly, only the averaged bonding state of an amount of particles is possible to be acquired using in situ XPS on few sites with synchrotron sources. In situ TEM-EELS makes the similar study available for every FEG TEM and even the chemical state of a single particle can be monitored. HRTEM images (below left) were taken at 300 °C with a resolution better than 1 Å (see FFT – below right) after the sample was reduced from CuO in 1 bar pressure of H2 + 4N2. EELS measurements were taken at 50 °C increments, showing that the reduction of CuO to metallic Cu is achieved at 250 °C. Experiment data from Dr. Qiang Xu, DENSsolutions, The Netherlands. |  |
Calorimetric analysis of CuO particle dynamicsExperiment: CuO exposed to 110 mBar MeOH at 500 °C The amount of heat absorbed or dissipated by the specimen during endo- or exo-thermic reactions can be determined with the highest accuracy using the Climate Nano-Reactor’s 4-point-probe micro-heater. A catalytic process usually contains several steps of reactions that generate or consume heat. Using constant temperature mode, the heat exchange within the Nano-Reactor can be measured for small but perceptible changes in the input power of the micro-heater. This exothermic behaviour was observed in the CuO redox experiment shown below where in situ TEM was used to observed the continuous phase transformations between Cu and Cu2O. The temperature set at 500 °C between 13:02 and 15:33 showed the reaction conditions as steady. As shown on the data sets below before 15:33, the temperature was oscillating around its mean value but power consumption was stable. However, just before 15:40 (shown below) no more oscillation of the temperature was observed and the power consumption of the Nano-Reactor suddenly decreases. Thereafter, the power signal shows irregular fluctuations with a decreasing trend over time. Although this phenomenon is not fully understood, it’s clear that there are exothermic reactions happening with no indication of change in relevant other parameters that would impact the power consumption of the heating spiral. Experiment data from Dr. Marc Willinger & Dr. Ramzi Farra, Fritz-Haber-Institute fur der Max-Planck-Gesellschaft, Germany. |  |
In situ Gas AnalyzerThe DENSsolutions Gas Analyzer is specifically designed to work seamlessly with the Climate in situ Gas & Heating solution. By enabling analysis of reaction products, it transforms the Climate into the only platform in the market able to combine TEM-based data with information about the kinetics of the reaction under examination. |  |
Climate EDS compatible nano-reactor
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Resolution
Pressure
Heating
Frequently Asked Questions
Is the Climate compatible with EDS and EELS?
What is the preparation time for a typical experiment?
- 5 minutes to load the sample on the Nano-Reactor (e.g. drop casting method and let the ethanol drop evaporate)
- 10 minutes to assemble the tip: placing the Nano-Reactor and closing off the lid
- 3 minutes to align the top chip membrane around the heater spiral on the bottom chip
- 10 minutes to do the electrical connection and leak test (pump down time taking most this time)
This time does not include sample preparation as this can vary from sample to sample.
What type of samples can be used inside the Climate Nano-Reactor?
What gases can be used in the Climate system?
- Silicon Nitride – Nano-Reactor’s window material
- Stainless Steel – Gas inlet lines, mass flow controllers, pressure gauges, control and mixing valves, pumps
- PEEK tubing – Fine tubing between Flow Control Unit and Sample Holder
- Fused Silica – Components in the Sample Holder
- Titanium – Sample Holder tip and lid
- Viton – Valve and controller seals in the Gas Supply System and O-rings sealing the Nano-Reactor
Any gases that can react with the above materials at room temperature (or at elevated temperatures for Silicon Nitride) should be avoided. If these gases are critical to your experiment, it is possible to dilute them to a safe level, however, this should be in consultation with DENSsolutions. Alternative materials for some components are possible, please contact DENSsolutions to discuss – e.g. Viton can be replaced by Kalrez. The mass flow controllers at the gas input lines of the Gas Supply System are calibrated for CxHy, O2, H2, N2, He, Ar, CO, CO2, Air. To know the exact gases that can be used, please refer to the chemical resistance sheet. For toxic gases the user will need to install additional safety features to monitor the concentration of that gas inside the lab room.
Is it necessary to use the Climate Gas-flow Supply System?
How long would it take to replace the gas tubing?
Can I safely use the Climate holder in my TEM?
Will the use of the Nano-Reactor have an impact on the analytical results?
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