Development of a Li-Ion Electrochemical Platform for in-Situ TEM of Solid State Electrode/Electrolyte Interfaces

Wednesday, 4 October 2017
Prince George's Exhibit Hall D/E (Gaylord National Resort and Convention Center)
R. Wang, J. S. Daubert (North Carolina State University), M. Ning, Y. Yang (Columbia University), Y. Liu, G. N. Parsons, E. C. Dickey, and V. Augustyn (North Carolina State University)
The interface of electrode materials in contact with solid-state electrolytes is of current interest for the development of devices with high energy density and good safety. In-situ transmission electron microscopy (TEM) of energy storage materials allows for the detailed study of structure-property relationships near solid interfaces during electrochemical charge and discharge. Here, we will describe the design of an in-situ TEM platform to investigate the structure-property relationship of a model energy storage oxide, V2O5, in contact with a state-of-the-art solid-state electrolyte Li7La3Zr2O12 (LLZO). The cell was fabricated by the atomic layer deposition (ALD) of V2O5 (~ 50 nm thick) onto the electrolyte and subsequent focused ion beam (FIB) milling and lift-out of a micron-long electrode/electrolyte architecture. The lithium metal anode was electrochemically deposited directly onto the gold electrode of an in-situ TEM chip. Assembly of the electrochemical cell was performed in a scanning electron microscope using a micromanipulator. Bright-field TEM and electron energy loss spectroscopy (EELS) showed that the deposited V2O5 layer formed a well-defined interface with LLZO and this allowed for the determination of the vanadium oxidation state. This work demonstrates the fabrication of a platform for the in-situ TEM study of materials at electrode/solid-state electrolyte interfaces that can readily be adapted to other types of solid state battery chemistries.