Analytical Chemistry

Data Synchronization in Operando Gas and Heating TEM



Time-resolved correlations between the environment, the reaction products, the energy transfer and the material structures during the reaction processes make operando gas and heating TEM more and more attractive in recent years. The intrinsic time delays that exist among parameter measurement locations need to be calibrated for valid correlations. Otherwise, erroneous conclusions would be drawn, such as over-estimating the critical temperatures, or mismatching the structure and composition relationships to activities. Herein, we report on a method measuring and calibrating the time delays involved in operando TEM. This method relies on the unique capability of on-chip calorimetry of the gas Nano-Reactor. It is shown that the time delay depends on the gas flow rate and pressure, and has little dependence on the gas type. A functional relationship fitted between the time delay and the gas flow rate can automize the time delay calibration and thus synchronize the data from different locations. Based on the investigations, we developed algorithms and scripts to enable the automatic data synchronization in operando gas and heating TEM in both real time experiments and post experiments.


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Supplementary material

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Data Synchronization in Operando Gas and Heating TEM Supplementary Information
The supplementary information for Data Synchronization in Operando Gas and Heating TEM. Including the time delays in ETEM, and the time delay between pre-TEM to in-TEM, and the figure of the relationship between time delay and pressure in Nano-Reactor.