Accurate control and measurement of real-time sample temperature are critical for the understanding and interpretation of the experimental results from in situ heating experiments inside environmental transmission electron microscope (ETEM). However, quantifying the real-time sample temperature remains a challenging task for commercial in situ TEM heating devices, especially under gas conditions. In this work, we developed a home-made micro-electrical-mechanical-system (MEMS) heater with unprecedented small temperature gradient and thermal drift, which not only enables the temperature evolution caused by gas injection to be measured in real-time but also makes the key heat dissipation path easier to model to theoretically understand and predict the temperature decrease. A new parameter termed as “gas cooling ability (H)”, determined purely by the physical properties of the gas, can be used to compare and predict the gas-induced temperature decrease by different gases. Our findings can act as a reference for predicting the real temperature for in situ heating experiments without closed-loop temperature sensing capabilities in the gas environment, as well as all gas-related heating systems.

In situ environmental transmission electron microscopy (ETEM) experiments require specimen heating holders to study material behavior in gaseous environments at elevated temperatures. In order to extract meaningful kinetic parameters, such as activation energies, it is essential to have a direct and accurate measurement of local sample temperature. This is particularly important if the sample temperature might fluctuate, for example when room temperature gases are introduced to the sample area. Using selected-area diffraction (SAD) in an ETEM, the lattice parameter of Ag nanoparticles was measured as a function of the temperature and pressure of hydrogen gas to provide a calibration of the local sample temperature. SAD permits measurement of temperature to an accuracy of ±30°C using Ag lattice expansion. Gas introduction can cause sample cooling of several hundred degrees celsius for gas pressures achievable in the ETEM.

This paper examines the reliability of a widely used method for temperature determination by multi-wavelength pyrometry. In recent warm dense matter experiments with ion-beam heated metal foils, we found that the statistical quality of the fit to the measured data is not necessarily a measure of the accuracy of the inferred temperature. We found a specific example where a second-best fit leads to a more realistic temperature value. The physics issue is the wavelength-dependent emissivity of the hot surface. We discuss improvements of the multi-frequency pyrometry technique, which will give a more reliable determination of the temperature from emission data.

Nous proposons une méthode d'estimation du flux de chaleur dans un outil de coupe lors d'une opération d'usinage par tournage et fraisage. Le modèle du comportement thermique de l'outil, reliant ce flux à la température mesurée en un point de l'outil, est obtenu au sens de l'identification de système non entier. Nous réalisons pour cela un dispositif de mesure de la température dans l'outil ainsi qu'un banc expérimental de caractérisation permettant de mesurer et de contrôler le flux de chaleur appliqué sur l'outil. Le modèle obtenu, après la phase d'identification des paramètres, permet de calculer la réponse impulsionnelle. Cette réponse est alors utilisée dans une procédure d'estimation séquentielle du flux.