Local temperature measurement in TEM by parallel beam electron diffraction

Niekiel, Florian; Kraschewski, Simon M.; Müller, Julian; Butz, Benjamin; Spiecker, Erdmann

doi:10.1016/j.ultramic.2016.11.028

Cited by 71 publications

(57 citation statements)

References 36 publications

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“…Vendelbo et al ., explored a quantitative electron energy loss spectroscopy (EELS) method that probes the local temperature of the spiral by measuring the local gas density. Niekiel et al . described local temperature measurements using parallel beam electron diffraction from TEM to map the temperature in MEMS devices, with in situ heating experiments in mind.…”

Section: Introductionsupporting

confidence: 87%

“…In both cases, a significant temperature gradient was found of 100°C in vacuum [32] and up to 320°C in air. [33] Although both EELS and electron diffraction experiments show potential for thermometry, the static environment and elaborate calibration procedure limit, in our view, the possibility for operando or in situ temperature measurements.…”

Section: Introductionmentioning

confidence: 96%

“…In this method, small gold nano‐particles were distributed over the surface and the temperature‐dependent diffraction rings, due to the thermal expansion of the nano‐particles, were investigated using selected area electron diffraction. In both cases, a significant temperature gradient was found of 100 °C in vacuum and up to 320 °C in air . Although both EELS and electron diffraction experiments show potential for thermometry, the static environment and elaborate calibration procedure limit, in our view, the possibility for operando or in situ temperature measurements.…”

Section: Introductionmentioning

confidence: 99%

“…Vendelbo et al, [32] explored a quantitative electron energy loss spectroscopy (EELS) method that probes the local temperature of the spiral by measuring the local gas density. Niekiel et al [33] described local temper- Figure 1. a) A schematic representation of the pathway of soft X-rays in scanning transmission X-ray microscopy (STXM).…”

Section: Introductionmentioning

confidence: 99%

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In Situ Local Temperature Mapping in Microscopy Nano‐Reactors with Luminescence Thermometry

et al. 2019

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In situ and operando experiments play a crucial role in understanding the mechanisms behind catalytic processes. In these experiments it is important to have precise control over pressure and temperature. In this work, we use luminescence thermometry to map the temperature distribution in a 300 μm microelectromechanical system nano‐reactor with a resolution of ca. 10 μm. These measurements showed a temperature gradient between the center and edge of the heater of ca. 200 °C (at Tset=600 °C) in vacuum and, in addition, a large offset of the local temperature of ca. 100 °C (at Tset=600 °C) in a non‐vacuum (i. e., air, He and H2) environment. The observed temperature heterogeneities can explain differences observed in the reduction behavior of Co‐based Fischer‐Tropsch synthesis catalyst particles at different locations in the nano‐reactor as determined by scanning transmission X‐ray microscopy.

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Section: Introductionsupporting

confidence: 87%

Section: Introductionmentioning

confidence: 96%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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In Situ Local Temperature Mapping in Microscopy Nano‐Reactors with Luminescence Thermometry

et al. 2019

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“…Even though in the present work, based on the experimental setup, e-beam irradiation is not expected to cause significant heating of the silica glass specimens, future work is planned to check this systematically as a case study. As shown just recently by Niekiel et al (2016), parallel beam electron diffraction can be used in situ in the TEM to perform local temperature measurements with high precision. A similar experimental setup is currently being developed to assess quantitative data of a possible temperature increase upon irradiation with electrons in the TEM.…”

Section: Membranes In the Temmentioning

confidence: 98%

A Novel Approach for Preparation and In Situ Tensile Testing of Silica Glass Membranes in the Transmission Electron Microscope

et al. 2017

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The mechanical behavior of glasses in the micro-and nanometer regime increasingly gains importance in nowadays modern technology. However, suitable small-scale preparation and mechanical testing approaches for a reliable assessment of the mechanical properties of glasses still remain a big challenge. In the present work, a novel approach for site-specific preparation and quantitative in situ tensile testing of thin silica glass membranes in the transmission electron microscope (TEM) is presented. Thereby, advanced focused ion beam techniques are used for the preparation of nanoscale dog bone-shaped silica glass specimens suitable for in situ tensile testing. Small amounts of gallium are detected on the surface of the membranes resulting from redeposition effects during the focused ion beam preparation procedure. Possible structural changes of silica glass upon irradiation with electrons and gallium ions are investigated by controlled irradiation experiments, followed by a structural analysis using Raman spectroscopy. While moderate electron beam irradiation does not alter the structure of silica glass, ion beam irradiation results in minor densification of the silica glass membranes. In situ tensile testing of membranes under electron beam irradiation results in distinctive elongations without fracture confirming the phenomenon of superplasticity. In contrast, in situ tensile testing in the absence of the electron beam reveals an elastic/plastic deformation behavior and finally leads to fracture of the membranes. The Young's moduli of the glass membranes pulled at beam-off conditions in the TEM are comparable with values known for bulk fused silica, while the tensile strength is in the range of values reported for silica glass fibers with comparable dimensions. The impact of electron beam irradiation on the mechanical properties of silica glass membranes is further discussed. The results of the present work open new avenues for dedicated preparation and nanomechanical characterization of silica glass and further contribute to a fundamental understanding of the mechanical behavior of such glasses when being scaled down to the nanometer regime.

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In‐Situ Transmission Electron Microscopy Experiments

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Local temperature measurement in TEM by parallel beam electron diffraction

Cited by 71 publications

References 36 publications

In Situ Local Temperature Mapping in Microscopy Nano‐Reactors with Luminescence Thermometry

In Situ Local Temperature Mapping in Microscopy Nano‐Reactors with Luminescence Thermometry

A Novel Approach for Preparation and In Situ Tensile Testing of Silica Glass Membranes in the Transmission Electron Microscope

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