Novel XRD technique and equipment for in-situ monitoring of phase transformations in lithium batteries during cycling

Full text: Safe, rechargeable batteries utilising a lithium metal electrode have not been realised due to phenomena, which occur on the lithium surface during the cycling of a battery. Lithium ion conduction inhomogeneities through the surface film give rise to uneven deposition of lithium, which can result in short circuits. The large potential increase in energy density that the use of the lithium electrode represents makes the nature of the surface film of interest to battery researchers. The lithium surface is highly reactive, particularly in the case of electrodes with a rough surface deposit. This presents difficulties to researchers hoping to obtain representative measurements of the lithium surface and requires the use of environmental sample chambers and in-situ techniques. X-ray diffraction techniques have been used to probe changes in cathode materials (typically transition metal oxides) for lithium batteries, but to our knowledge has not been successfully used to study changes taking place on the lithium surface during cycling. We present early results from work we have undertaken to develop a technique for characterising the surface film on lithium battery electrodes. The instrumentation was set-up as follows. An XRD was fitted with an INEL CPS 120 position sensitive detector (PSD), multilayer mirror and environmental chamber. The latter was specially developed in our laboratory for the purpose of these experiments. The lithium cells were sealed in laminated foil. Cycled and uncycled cells were investigated. Different radiation sources were used (Cu, Co and Cr). The in-situ measurements aiming at monitoring the phase transitions of cycled/uncycled cells at different angles (including grazing angles) in time were carried out in both transmission and reflection mode. Copyright (2002) Australian X-ray Analytical Association Inc