XRD evidence of macroscopic composition inhomogeneities in the graphite–lithium electrode

In situ and ex situ X-ray diffraction (XRD) measurements were carried out on lithiated graphite electrodes at different states of charge. Data were collected from both sides of electrode. We found macroscopic inhomogeneities in the lithium concentration along the electrode thickness even when the electrode was allowed to rest for 24 h. The electrode side facing the lithium counter electrode in the coin type half-cell displays higher lithium concentration as compared to the side opposed to the XRD window. Residual stage 2 compound is found in the supposedly fully lithiated and fully delithiated electrode. It seems that the differences in the chemical potential between stage 2 and stage 1 is too small to average the lithium composition through chemical diffusion at ambient temperature in reasonable times.