Exploring the influence of FIB processing and SEM imaging on solid-state electrolytes.

Performing reliable preparation of TEM samples is the necessary basis for a meaningful investigation by ex-situ and even more so by in-situ TEM techniques, but it is challenging using materials that are sensitive to electron-beam irradiation. FIB is currently the most commonly employed technique for a targeted preparation, but the structural modifications induced during FIB preparation are not fully understood for a number of materials. Here, we have investigated the impact of both the electron and the Ga+ ion beam on insulating solid-state electrolytes (LiPON, BASE and NaSICON) and observed significant Li/Na whisker growth induced by both the electron and ion beam already at fairly low dose leading to a significant change in the chemical composition. The metal whisker growth is presumably mainly due to surface charging which can be reduced by coating with a gold layer or preparation at cryogenic conditions as efficient approaches to stabilize the solid electrolyte for SEM imaging and TEM sample preparation. Details on the different preparation approaches, the acceleration voltage dependence and the induced chemical and morphological changes are reported.

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