skip to main content


Title: Quantifying Real-Time Sample Temperature Under the Gas Environment in the Transmission Electron Microscope Using a Novel MEMS Heater
Abstract 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.  more » « less
Award ID(s):
1905647
PAR ID:
10386173
Author(s) / Creator(s):
; ; ; ;
Date Published:
Journal Name:
Microscopy and Microanalysis
Volume:
27
Issue:
4
ISSN:
1431-9276
Page Range / eLocation ID:
758 to 766
Format(s):
Medium: X
Sponsoring Org:
National Science Foundation
More Like this
  1. Abstract

    Ferroelectrics, due to their polar nature and reversible switching, can be used to dynamically control surface chemistry for catalysis, chemical switching, and other applications such as water splitting. However, this is a complex phenomenon where ferroelectric domain orientation and switching are intimately linked to surface charges. In this work, the temperature‐induced domain behavior of ferroelectric‐ferroelastic domains in free‐standing BaTiO3films under different gas environments, including vacuum and oxygen‐rich, is studied by in situ scanning transmission electron microscopy (STEM). An automated pathway to statistically disentangle and detect domain structure transformations using deep autoencoders, providing a pathway towards real‐time analysis is also established. These results show a clear difference in the temperature at which phase transition occurs and the domain behavior between various environments, with a peculiar domain reconfiguration at low temperatures, from a‐c to a‐a at ≈60 °C. The vacuum environment exhibits a rich domain structure, while under the oxidizing environment, the domain structure is largely suppressed. The direct visualization provided by in situ gas and heating STEM allows to investigate the influence of external variables such as gas, pressure, and temperature, on oxide surfaces in a dynamic manner, providing invaluable insights into the intricate surface‐screening mechanisms in ferroelectrics.

     
    more » « less
  2. Abstract

    Reactive flash sintering has been demonstrated as a method to rapidly densify and synthesize ceramic materials, but determining the extent of chemical reactions can be complex since the maximum temperature reached by the sample may be brief in time. The black body radiation (BBR) model has been shown to accurately predict the sample temperature during the steady state of flash (stage III). This work demonstrates situations where the BBR model alone does not accurately predict when a phase transformation will occur. We examine the model reactions of CuO reduction to Cu2O during stage II and Mn2O3reduction to Mn3O4in stage III. In CuO, highly resistive samples result in initially localized current flow, a stochastic process resulting in inhomogeneous heating and error in the BBR model during stage II. CuO reduction does not occur in constant heating rate experiments with 6.25 V/mm fields, even though the sample temperature momentarily exceeds the phase transformation temperature. Increased furnace heating to 950°C before application of a field is required to drive the transition. In Mn2O3, the calculated sample temperature of the gauge is less than the transformation temperature, but localized heating at the contact will exceed the transformation temperature, causing the transformation to propagate away from the electrode during stage III. This work demonstrates two forms of inhomogeneity (local, stochastic current flow, and local contact resistance) that result in a complex thermal profile of the sample. This profile should be interrogated to understand reaction kinetics, and can be beneficial when engineered.

     
    more » « less
  3. Knowledge of the kinetic behavior of He in apatite and other U- and Th-bearing minerals comes largely from detailed step-heating experiments, yet such experiments are time consuming and are rarely performed during routine thermochronological studies using the U-Th/He method. We propose a new analytical method for measuring both the bulk 4He abundance and the kinetics of He release in apatite. Using this method He is extracted from samples by continuous heating using a ramped temperature schedule under static vacuum conditions, and the evolved He is measured periodically as it accumulates in the extraction system. Continuous ramped heating (CRH) experiments can be conducted using instrumentation available in most noble-gas ther- mochronology labs but require particular attention to temperature control, measurement linearity and dynamic range, and suppression of active gases co-evolved with He. CRH experiments require little more time than conventional single-step heating measurements but yield a detailed record of He release not provided by con- ventional methods. Kinetic parameters for He diffusion in Durango apatite derived from continuous heating data agree well with those obtained from published step-heating studies. The continuous record of He release ob- tained from CRH experiments also provides important information about the siting of He and the presence of multiple He components in apatite, some of which may be responsible for anomalous U-Th/He ages and high age dispersion. As such the CRH method shows promise as a useful sample screening tool for apatite U-Th/He thermochronology. 
    more » « less
  4. Recent studies have established immersive virtual environments (IVEs) as promising tools for studying human thermal states and human–building interactions. One advantage of using immersive virtual environments is that experiments or data collection can be conducted at any time of the year. However, previous studies have confirmed the potential impact of outdoor temperature variations, such as seasonal variations on human thermal sensation. To the best of our knowledge, no study has looked into the potential impact of variations in outdoor temperatures on experiments using IVE. Thus, this study aimed to determine if different outdoor temperature conditions affected the thermal states in experiments using IVEs. Experiments were conducted using a head mounted display (HMD) in a climate chamber, and the data was analyzed under three temperature ranges. A total of seventy-two people participated in the experiments conducted in two contrasting outdoor temperature conditions, i.e., cold and warm outdoor conditions. The in situ experiments conducted in two cases, i.e., cooling in warm outdoor conditions and heating in cold outdoor conditions, were used as a baseline. The baseline in-situ experiments were then compared with the IVE experiments conducted in four cases, i.e., cooling in warm and cold outdoor conditions and heating in warm and cold outdoor conditions. The selection of cooling in cold outdoor conditions and heating in warm outdoor conditions for IVE experiments is particularly for studying the impact of outdoor temperature variations. Results showed that under the experimental and outdoor temperature conditions, outdoor temperature variations in most cases did not impact the results of IVE experiments, i.e., IVE experiments can replicate a temperature environment for participants compared to the ones in the in situ experiments. In addition, the participant’s thermal sensation vote was found to be a reliable indicator between IVE and in situ settings in all studied conditions. A few significantly different cases were related to thermal comfort, thermal acceptability, and overall skin temperature. 
    more » « less
  5. ABSTRACT

    We study the properties of cosmic-ray (CR) driven galactic winds from the warm interstellar medium using idealized spherically symmetric time-dependent simulations. The key ingredients in the model are radiative cooling and CR-streaming-mediated heating of the gas. Cooling and CR heating balance near the base of the wind, but this equilibrium is thermally unstable, leading to a multiphase wind with large fluctuations in density and temperature. In most of our simulations, the heating eventually overwhelms cooling, leading to a rapid increase in temperature and a thermally driven wind; the exception to this is in galaxies with the shallowest potentials, which produce nearly isothermal $T \approx 10^4\,$ K winds driven by CR pressure. Many of the time-averaged wind solutions found here have a remarkable critical point structure, with two critical points. Scaled to real galaxies, we find mass outflow rates $\dot{M}$ somewhat larger than the observed star-formation rate in low-mass galaxies, and an approximately ‘energy-like’ scaling $\dot{M} \propto v_{\rm esc}^{-2}$. The winds accelerate slowly and reach asymptotic wind speeds of only ∼0.4vesc. The total wind power is $\sim 1~{{\ \rm per\ cent}}$ of the power from supernovae, suggesting inefficient preventive CR feedback for the physical conditions modelled here. We predict significant spatially extended emission and absorption lines from 104–105.5 K gas; this may correspond to extraplanar diffuse ionized gas seen in star-forming galaxies.

     
    more » « less