MXenes are an emerging family of highly-conductive 2D materials which have demonstrated state-of-the-art performance in electromagnetic interference shielding, chemical sensing, and energy storage. To further improve performance, there is a need to increase MXenes’ electronic conductivity. Tailoring the MXene surface chemistry could achieve this goal, as density functional theory predicts that surface terminations strongly influence MXenes' Fermi level density of states and thereby MXenes’ electronic conductivity. Here, we directly correlate MXene surface de-functionalization with increased electronic conductivity through in situ vacuum annealing, electrical biasing, and spectroscopic analysis within the transmission electron microscope. Furthermore, we show that intercalation can induce transitions between metallic and semiconductor-like transport (transitions from a positive to negative temperature-dependence of resistance) through inter-flake effects. These findings lay the groundwork for intercalation- and termination-engineered MXenes, which promise improved electronic conductivity and could lead to the realization of semiconducting, magnetic, and topologically insulating MXenes.

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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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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