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Performing In Situ Closed-Cell Gas Reactions in the Transmission Electron Microscope
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Data synchronization in operando gas and heating TEM.

Fan Zhang1, Merijn Pen2, Ronald G Spruit2

  • 1Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics (DICP), Chinese Academy of Sciences, Dalian, China; University of Chinese Academy of Sciences, Beijing, China.

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|May 18, 2022
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Summary

Accurate operando transmission electron microscopy (TEM) requires synchronizing measurements. This study presents a novel method using on-chip calorimetry to calibrate time delays, ensuring reliable correlations between material structure and reaction conditions.

Keywords:
Automatic characterization and calibrationData synchronizationOperando TEMTime delay

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Physical Chemistry

Background:

  • Operando gas and heating transmission electron microscopy (TEM) is increasingly vital for studying reaction dynamics.
  • Accurate time-resolved correlations require calibration of time delays between different measurement points.
  • Existing methods risk erroneous conclusions regarding critical temperatures and structure-activity relationships due to uncalibrated delays.

Purpose of the Study:

  • To develop and validate a method for synchronizing data from pre-, in-, and post-TEM measurements.
  • To address the critical need for precise time-delay calibration in operando TEM experiments.

Main Methods:

  • Utilized on-chip calorimetry within a gas Nano-Reactor, intrinsically synchronized with TEM imaging and spectroscopy.
  • Measured and calibrated time delays between different parameter measurement locations.
  • Developed a functional relationship between time delay, gas flow rate, and pressure for automated calibration.

Main Results:

  • Successfully synchronized data from multiple measurement locations in operando gas and heating TEM.
  • Identified time delay dependence on gas flow rate and pressure, with minimal dependence on gas type.
  • Developed algorithms and scripts for automated, real-time, and post-experiment data synchronization.

Conclusions:

  • The developed method ensures accurate time-resolved correlations in operando TEM.
  • Automated calibration based on gas flow rate and pressure enhances experimental reliability.
  • This approach enables more precise understanding of material behavior during reactions.