A novel fabrication technique, namely electrostatic spray deposition (
ESD), has been developed in order to prepare thin layers of solid elec
trolytes and cathode materials for lithium batteries. In this study, t
he 4-volt cathode material LiCoO2 was chosen, and prepared by spraying
alcohol solutions of nitrates and acetates of cobalt. ESD set-ups, wi
th either horizontal or Vertical configurations, were used. Depending
on the precursor and process deposition conditions, the morphology of
the layers can be relatively dense, fractal-like porous, or unique 3-D
cross-linked porous structures with a high porosity and a narrow pore
size distribution. For low deposition temperatures, LiCoO2 layers are
XRD amorphous. Upon annealing, crystallized layers are obtained. The
lithium chemical diffusion coefficient of the LiCoO2 layers has been m
easured with Galvanostatic Intermittent Titration Technique (GITT), va
lues range from 10(-14) to 10(-12) cm(2)/s, depending on the lithium c
ontent and the annealing temperatures. Cyclic Voltammograms of a test
cell reveal that both lithium insertion and extraction are one-step pr
ocesses.