The present study focuses on the characterization of non-structured and laser modified films before and after electrochemical cycling using a combination of complementary surface analytical methods. For this purpose rf magnetron sputtered lithium cobalt oxide and lithium manganese oxide were structured with laser radiation leading to a surface microstructure with increased active surface area. In particular, high repetition excimer laser radiation with a pulse width of 4-6 nm and 248 nm wavelength was used. Self-organized conical microstructures were formed using laser fluences between 0.5 J/cm² and 2.0 J/cm². A subsequent annealing process using high power diode laser radiation at 940 nm wavelength enables the adjustment of the required crystallinity.

X-ray photoelectron spectroscopy (XPS) provides the chemical composition in a non-destructive manner. The in-depth distribution of the electrode constituents and the solid electrolyte interface after cycling was studied by time-of-flight secondary mass spectrometry (ToFSIMS) and XPS sputter depth profiles. In addition, the conical topography was shown by scanning electron microscopy (SEM) and crystallinity was proven by X-ray diffraction.