Data synchronization in operando gas and heating TEM

Abstract

Time-resolved correlations of 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 time delays existing among parameter measurement locations need to be calibrated for valid correlations. Otherwise, erroneous conclusions would be drawn, such as over/under-estimating the critical temperatures, mismatching the structure and composition relationships to activities, and so on. Herein, we report on a method synchronizing the data from pre-, in- and post-TEM by measuring and calibrating the time delays involved. This method relies on the unique capability of on-chip calorimetry of the gas Nano-Reactor, which is intrinsically synchronized with the TEM imaging and spectroscopy data. The time delay is found to be dependent on the gas flow rate and pressure, and have little dependence on the gas type. A functional relationship fitted between the time delay and the gas flow rate and pressure can automate 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.