In-situ Transmission Electron Microscopy Characterization of Electrochemical Processes in Solid-state Energy Storage Devices with Air Sensitive Materials

Fundamental scientific advances are needed to create breakthrough materials that will improve the performance of electrical and energy storage devices. Over the last decade in- situ transmission electron microscopy (TEM) has been used to characterize these materials in devices at resolutions down to the atomic level. Importantly, this can also be done at the same time that the devices are operating (operando). This allow direct correlations to be made between material structure and device performance. However, for materials that are sensitive to air-exposure – e.g. Li battery materials, where exposure to air for even a few seconds can significantly affect material structure and chemistry – researchers currently do not have an adequate solution to transfer samples from a protective preparation environment (e.g. a glove box) into the TEM without exposing the samples to air. As a result, any of these experiments could be questioned on the basis that it is not known what the effect of air-exposure is on the materials that are being characterized. This proposal will solve this challenge by developing and bringing to market a transmission electron microscopy vacuum/inert-gas transfer electrical biasing and heating specimen holder that will allow routine imaging of the nanoscale physics and chemistry occurring within operating electronic and energy storage devices and at the same time allowing air-free transfer of sample into the TEM. The broader impact/commercial potential of this project will be that when we take away the major obstacle of air-free transfer in performing these in-situ TEM experiments, this will allow researchers and technologists to rapidly advance the fundamental understanding of these processes, to make better-informed decisions regarding optimum materials and designs, and to thereby accelerate the manufacture of next generation electrical device technologies. The issue of air-free handling is very important especially in the areas of catalysis and energy storage materials, because of the sensitivity that these materials display to exposure to oxygen or moisture. Furthermore, many of the nanoscale semiconductor systems have a high sensitivity to oxygen as it dopes the structures or changes the defect density, so air free handling in preparation of any (in-situ) TEM imaging is very important. It is also important for the 2D semiconducting systems and "Quantum Materials" systems that are a big push within research currently funded by DOE.