Recent advances in energy materials have led to the development of high capacity insertion cathodes for Li-ion batteries. A relatively new, yet attractive material is nickel cobalt aluminium oxide (NCA). However, lithium diffusion has yet to be experimentally characterised on a local scale for NCA, a highly attractive material for commercial applications. Thus, this study proposes investigation into the lithium diffusion properties in NCA for the first time and compare these to the bulk lithium diffusion observed from other techniques such as EIS and CV. The effect of particle size will also be studied.