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In-Situ Characterization of Lithium Native Passivation Layer in A High Vacuum Scanning Electron Microscope

Published online by Cambridge University Press:  24 May 2019

Stéphanie Bessette ,
Pierre Hovington ,
Hendrix Demers ,
Maryam Golozar ,
Patrick Bouchard ,
Raynald Gauvin  and
Karim Zaghib Open the ORCID record for Karim Zaghib [Opens in a new window]
Stéphanie Bessette
Affiliation:
Hydro-Québec, Center of Excellence in Transportation Electrification and Energy Storage, Varennes, J3X 1S1, Canada McGill University, Department of Mining and Materials Engineering, Montréal, H3A 0C5, Canada
Pierre Hovington
Affiliation:
Consulting Hovington, Boucherville, Québec, Canada
Hendrix Demers
Affiliation:
Hydro-Québec, Center of Excellence in Transportation Electrification and Energy Storage, Varennes, J3X 1S1, Canada
Maryam Golozar
Affiliation:
Hydro-Québec, Center of Excellence in Transportation Electrification and Energy Storage, Varennes, J3X 1S1, Canada McGill University, Department of Mining and Materials Engineering, Montréal, H3A 0C5, Canada
Patrick Bouchard
Affiliation:
Hydro-Québec, Center of Excellence in Transportation Electrification and Energy Storage, Varennes, J3X 1S1, Canada
Raynald Gauvin
Affiliation:
McGill University, Department of Mining and Materials Engineering, Montréal, H3A 0C5, Canada
Karim Zaghib*
Affiliation:
Hydro-Québec, Center of Excellence in Transportation Electrification and Energy Storage, Varennes, J3X 1S1, Canada
*
*Author for correspondence: Karim Zaghib, E-mail: [email protected]
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Abstract

A technique to characterize the native passivation layer (NPL) on pure lithium metal foils in a scanning electron microscope (SEM) is described in this paper. Lithium is a very reactive metal, and consequently, observing and quantifying its properties in a SEM is often compromised by rapid oxidation. In this work, a pure lithium energy-dispersive x-ray spectrum is obtained for the first time in a high vacuum SEM using a cold stage/cold trap with liquid nitrogen reservoir outside the SEM chamber. A nanomanipulator (OmniProbe 400) inside the microscope combined with x-ray microanalysis and windowless energy dispersive spectrometer is used to fully characterize the NPL of lithium metal and some of its alloys by a mechanical removal procedure. The results show that the native films of pure lithium and its alloys are composed of a thin (25 nm) outer layer that is carbon-rich and an inner layer containing a significant amount of oxygen. Differences in thickness between laminated and extruded samples are observed and vary depending on the alloy composition.

Keywords

energy dispersive x-ray spectrometry (EDS)lithium metalnative passivation layerscanning electron microscopy (SEM)solid electrolyte interface (SEI)
Type
Materials Applications
Information
Microscopy and Microanalysis , Volume 25 , Issue 4 , August 2019 , pp. 866 - 873
Copyright
Copyright © Microscopy Society of America 2019 

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