Highly sensitive operando pressure measurements of Li-ion battery materials with a simply modified Swagelok cell

Abstract

A new cell design has been developed using a standard Swagelok cell for Li-ion battery material characterisation, which has been modified by replacing one of the electrode cylindrical plungers with an adaptor to a pressure sensor. By simplifying the cell design (no valves or unnecessary connectors have been included), the cell headspace volume is kept at a minimum (ca. 1.9 ml for a one-inch-diameter cell) which produces a dramatic increase in sensitivity of the measurements with respect to conventional set-ups. Changes in pressure induced by Li-ion battery materials processes (gas evolution, structural changes in volume of the battery material due to Li-ion insertion/extraction) are monitored with unprecedented sensitivity. Here we illustrate the application of this novel cell design for the operando pressure measurements of LiFePO4 and graphite in Li half-cell configurations, and detailed procedures of cell calibration, protocols for cell preparation and assembly and technical drawings of the cell parts are provided to facilitate the adoption of this technique for testing new battery materials. We also demonstrate the high sensitivity of this new set-up to study the corrosion of cell materials in contact with LiPF6-containing electrolytes, which had not been explored before with operando pressure measurements.

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ORCID for Nuria Garcia-Araez: orcid.org/0000-0001-9095-2379

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