AVS 65th International Symposium & Exhibition
    Applied Surface Science Division Monday Sessions
       Session AS-MoA

Paper AS-MoA1
Overcoming Obstacles in Surface and Interface Characterization of All Solid-State Lithium Battery Materials

Monday, October 22, 2018, 1:20 pm, Room 204

Session: Multitechnique Applications-When More techniques are Better than One
Presenter: Natalie Seitzman, Colorado School of Mines
Authors: N. Seitzman, Colorado School of Mines
H. Guthrey, National Renewable Energy Laboratory
D. Sulas, National Renewable Energy Laboratory
S. Johnston, National Renewable Energy Laboratory
J. Nelson Weker, SLAC National Accelerator Laboratory
H. Platt, Solid Power, Inc.
M. Al-Jassim, National Renewable Energy Laboratory
S. Pylypenko, Colorado School of Mines
Correspondent: Click to Email

Novel battery technologies are a key route to sustainable energy, but new chemistries come with new failure mechanisms that present characterization challenges. The nature of many promising next-generation batteries makes them inherently difficult to study, and multiple techniques must be combined to capture the relevant phenomena. For all-solid-state lithium batteries, one challenge is the reactivity of the battery components restrict which types of techniques may be used. Additionally, although the interfaces are of great interest, processes that expose them for characterization have unknown, likely deleterious effects on their integrity. Therefore, in order to understand characterization of surfaces and interfaces in batteries, bulk characterization and in situ characterization at multiple scales is also needed.

The focus of this work is probing the morphological evolution, including dendrite formation, of the electrode-electrolyte interface between lithium metal and β-Li3PS4 solid electrolyte. This is done through a combination of lock-in thermography, x-ray tomography, in situ scanning electron microscopy (SEM), and x-ray absorption near edge structure (XANES). We used thermography as a first step to identify trends in location of dendritic features, to guide techniques with smaller fields of view and greater resolution, such as SEM. X-ray tomography enables characterization of the interfaces without deconstructing the device or exposing the interfaces needed for surface characterization. Therefore, micro-tomography was performed both to study morphological changes and to check that results observed in other experiments with modified samples—such as nano-tomography, which required a focused ion beam to cut and lift out micron-scale samples—are consistent with the behavior of unaltered materials. In situ SEM cycling experiments and windowless energy dispersive spectroscopy (EDS) provided morphological and chemical characterization of the changing surfaces and interfaces with high spatial resolution. Detailed chemical characterization of the bulk material was obtained with XANES at the sulfur and phosphorus K-edges. This work furthers the development of surface and interface characterization of battery materials and moves toward localized, nanoscale characterization.