Towards optimization of experimental parameters for studying Li-O2 battery discharge products in TEM using in situ EELS

The key to understanding the performance of Li-O-2 batteries is to study the chemical and structural properties of their discharge product(s) at the nanometer scale. Using TEM for this purpose poses challenges due to the sensitivity of samples to air and electron beams. This paper describes our use of in situ EELS to evaluate experimental procedures to reduce electron-beam degradation and presents methods to deal with air sensitivity. Our results show that Li2O2 decomposition is dependent on the total dose and is approximately 4-5 times more pronounced at 80 than at 200 kV. We also demonstrate the benefits of using low-dose-rate STEM. We show further that a "graphene cell", which encapsulates the sample within graphene sheets, can protect the sample against air and e-beam damage. (C) 2018 Elsevier B.V. All rights reserved.