Advanced microheater for in situ transmission electron microscopy; enabling unexplored analytical studies and extreme spatial stability

Omme, J. Tijn van; Zakhozheva, Marina; Spruit, Ronald G.; Sholkina, Mariya; Garza, Héctor Hugo Pérez

doi:10.1016/j.ultramic.2018.05.005

Cited by 59 publications

(53 citation statements)

References 45 publications

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“…2b). We observed no change in performance with activation of the MEMS heater during experiments up to temperatures of 823 K. In line with our measurements, the temperature stability, precision, control, and uniformity in similar MEMS chips are well documented up to the maximum temperatures, usually ~1073 K (800°C) (Allard et al, 2009; Mele et al, 2016; Perez-Garza et al, 2016; van Omme et al, 2018; Gaulandris et al, 2020). Cooled to the cryogenic baseline of ~100 K without MEMS heating (Fig.…”

Section: Resultssupporting

confidence: 88%

Atomic-Resolution Cryo-STEM Across Continuously Variable Temperatures

et al. 2020

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Atomic-resolution cryogenic scanning transmission electron microscopy (cryo-STEM) has provided a path to probing the microscopic nature of select low-temperature phases in quantum materials. Expanding cryo-STEM techniques to broadly tunable temperatures will give access to the rich temperature-dependent phase diagrams of these materials. With existing cryo-holders, however, variations in sample temperature significantly disrupt the thermal equilibrium of the system, resulting in large-scale sample drift. The ability to tune the temperature without negative impact on the overall instrument stability is crucial, particularly for high-resolution experiments. Here, we test a new side-entry continuously variable temperature dual-tilt cryo-holder which integrates liquid nitrogen cooling with a 6-pin micro-electromechanical system (MEMS) sample heater to overcome some of these experimental challenges. We measure consistently low drift rates of 0.3–0.4 Å/s and demonstrate atomic-resolution cryo-STEM imaging across a continuously variable temperature range from ~100 K to well above room temperature. We conduct additional drift stability measurements across several commercial sample stages and discuss implications for further developments of ultra-stable, flexible cryo-stages.

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Section: Resultssupporting

confidence: 88%

Atomic-Resolution Cryo-STEM Across Continuously Variable Temperatures

et al. 2020

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“…The microheater consists of a spiral-shaped metal that is embedded between two layers of silicon nitride that form a membrane ( Figure 1 a,b). 24 A silicon substrate supports the membrane with the microheater and enables loading into a dedicated TEM holder. Four metal needles connect the holder with the metal contacts of the microheater.…”

Section: Resultsmentioning

confidence: 99%

Mapping Elevated Temperatures with a Micrometer Resolution Using the Luminescence of Chemically Stable Upconversion Nanoparticles

Swieten

Omme

Heuvel

et al. 2021

ACS Appl. Nano Mater.

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The temperature-sensitive luminescence of nanoparticles enables their application as remote thermometers. The size of these nanothermometers makes them ideal to map temperatures with a high spatial resolution. However, high spatial resolution mapping of temperatures >373 K has remained challenging. Here, we realize nanothermometry with high spatial resolutions at elevated temperatures using chemically stable upconversion nanoparticles and confocal microscopy. We test this method on a microelectromechanical heater and study the temperature homogeneity. Our experiments reveal distortions in the luminescence spectra that are intrinsic to high-resolution measurements of samples with nanoscale photonic inhomogeneities. In particular, the spectra are affected by the high-power excitation as well as by scattering and reflection of the emitted light. The latter effect has an increasing impact at elevated temperatures. We present a procedure to correct these distortions. As a result, we extend the range of high-resolution nanothermometry beyond 500 K with a precision of 1–4 K. This work will improve the accuracy of nanothermometry not only in micro- and nanoelectronics but also in other fields with photonically inhomogeneous substrates.

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“…The metal heating coil resistance is linearly dependent on the temperature, which allows for simultaneous heating and accurate temperature measurement 56. In this way the software is able to control the temperature via a closed loop feedback algorithm, similar to our previous efforts for in situ heating in vacuum or gas 48,57. In this case the heater is not located on a membrane close to the imaging area but on the silicon substrate instead(Figure 2).…”

mentioning

confidence: 96%