Investigating materials while changing temperature expands the application space of conventional TEM and enhances its already powerful imaging capabilities.
The Wildfire system allows for researchers to heat from room temperature to 1,300 °C with the ultimate temperature control and ultimate sample stability in all directions.
The stability of the Wildfire system ensures that the full resolution and analytical performance of every TEM can be maintained while observing sample dynamics at elevated temperature.
Obtaining the ‘game changing’ experimental results is the goal of any researcher – academic or industry. The team at Cambridge University focusing on energy related materials used the Wildfire system to study perovskite solar cells and their degradation processes during heating. These solar cells have become increasingly popular, however, the stability and lifetime of such devices at elevated temperatures are of concern. In situ TEM was used to understand the changes in morphology and chemical composition, leading to an improved understanding of the degradation evolution and Nature Energy publication.
Heat-induced degradation of perovskite solar cells. G. Divitini, et al. University of Cambridge Nature Energy 2016. DOI: 10.1038/nenergy.2015.12123
Behavior at the macroscale is strongly linked to atomic arrangement and its transformation. In this example Ru nanoparticles supported on silica are heated to 1300 °C using a DENSsolutions Wildfire system. At that temperatures, the SiO2 sphere evaporates and the Ru nanoparticles become very mobile. The emphasized nanoparticle changes from round to square. This shape change can be studied in detail, due to technology behind DENSsolutions heating systems which ensures high sample stability, sub-Å resolution and therefore enables deeper understanding of the processes involved.
Courtesy of Gatan. Acquired with Wildfire D6 (now H+ DT) and Gatan OneView IS camera on a Thermo Fisher Scientific (FEI) Tecnai TF20
Chemical analysis while heating is extremely important to understand the dynamics of temperature-induced transformations High quality EDS analysis at elevated temperatures is challenging due to the intense generation of infrared radiation during heating which disturbs the X-Ray spectral acquisition. DENSsolutions provides the technology and the experimental evidence that in situ EDS at elevated temperatures is reliable and robust technique across a large temperature range. For the first time it was shown that EDS analysis is possible even at 1000 °C.
Acquired on a Wildfire S3. Maps courtesy of Bruker
The closed 4-point probe feedback loop provides maximum versatility, accuracy (95%) and temperature uniformity (99.5%) in controlling stimuli and measuring responses.
Precise control at all temperatures is achieved through four-probe heating, with temperature stability deviations of less than 0.005°C; temperature uniformity deviations of less than 0.5%; and direct customer verification of temperatures in transmission electron microscopy (TEM) using EELS and SAED techniques.
Even at temperatures up to 1000C (AT=1000C), the drift rate is less than 200nm, the sample stabilization time is short, and the atomic level resolution can be achieved even at high voltages.
Optimal temperature uniformity: The window is located in the center of the miniature heater for the highest temperature uniformity, which can be as high as 99%. In addition, the surrounding metal further reduces electrostatic effects.
FIB lamellas: The circular shape of these windows and the absence of topography around these windows make them ideal for positioning.
High tilting: The elongated windows, placed perpendicular to the alpha tilt axis, offer optimal sample visibility at high tilt angles, perfect for tomography.
o far bulging (height change of the membrane while changing temperature and therefore blurred images) was unavoidable.. The Nano-Chip design reduces the bulging phenomenon.
WildfireModular design for stability and reliability
 Compatible with mini-pole gap
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 Double tilt
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 Mechanical Stability
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 EDS Optimized
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The sample holder brings the Wildfire Nano-chip into the TEM. samples are made of material with optimal mechanical stability and are designed for direct integration into ThermoFisher or JEOL microscopes.
| JEOL | Thermo Fisher Scientific | |
| Heating control | Closed 4-point probe feedback loop | Closed 4-point probe feedback loop |
| Temperature range | RT - 1,300 °C | RT - 1,300 °C |
| Polepiece compatibility | All | Bio-TWIN, C-TWIN, TWIN, X-TWIN, S-TWIN |
| Alpha tilt range | URP, FHP ≥ ± 15 deg HRP, WGP ≥ ± 20 deg | ≥ ± 25 deg |
| Beta tilt range | URP, FHP ≥ ± 15 deg HRP, WGP ≥ ± 25 deg | ≥ ± 25 deg |
| Attainable resolution* | ≤ 60 pm | ≤ 60 pm |
| Drift rate* | ≤ 0.5 nm/min | ≤ 0.5 nm/min |
| Temperature accuracy | ≥ 95 % | ≥ 95 % |
| Temperature Homogeneity | ≥ 99.5 % | ≥ 99.5 % |
| Viewable area | 850 µm2 | 850 µm2 |
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Low Dimensional Materials -
Nanotechnology -
Materials Engineering -
Materials Energy Applications -
Soft Matter Systems
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“In-situ TEM provides a new dimension in dynamic structural studies of a range of technologically important materials. The Department of Materials at Oxford will use the DENSsolutions sample heating holder in a number of projects related to catalysis and low dimensional carbon materials. We have chosen this solution for its unrivaled stability and control.”
Angus Kirkland Professor of Materials University of Oxford, United Kingdom -
“The DENSsolutions holder impressed me with high resolution imaging and extreme stability at high temperatures. It is exciting that the picture taken with the DENSsolutions holder shows superior performance compared to other holders. As long as we have got the DENSsolutions holder, we have got the in-situ world spinning in our hand.”
Professor Xiaoyan Zhong Tsinghua University Beijing, China -
“In-situ Transmission Electron Microscopy is one of the most exciting avenues for future breakthroughs in the characterization of dynamic processes in nano scale materials and devices. The DENSsolutions sample heating systems have performed impressively in experiments carried out in the Ernst Ruska-Centre.”
Professor Rafal Dunin-Borkowski Director, Ernst Ruska-Centre (ER-C) Forschungezentrum Jülich, Germany
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“In-situ TEM provides a new dimension in dynamic structural studies of a range of technologically important materials. The Department of Materials at Oxford will use the DENSsolutions sample heating holder in a number of projects related to catalysis and low dimensional carbon materials. We have chosen this solution for its unrivaled stability and control.”
Angus Kirkland Professor of Materials University of Oxford, United Kingdom -
“The DENSsolutions holder impressed me with high resolution imaging and extreme stability at high temperatures. It is exciting that the picture taken with the DENSsolutions holder shows superior performance compared to other holders. As long as we have got the DENSsolutions holder, we have got the in-situ world spinning in our hand.”
Professor Xiaoyan Zhong Tsinghua University Beijing, China -
“In-situ Transmission Electron Microscopy is one of the most exciting avenues for future breakthroughs in the characterization of dynamic processes in nano scale materials and devices. The DENSsolutions sample heating systems have performed impressively in experiments carried out in the Ernst Ruska-Centre.”
Professor Rafal Dunin-Borkowski Director, Ernst Ruska-Centre (ER-C) Forschungezentrum Jülich, Germany
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