were obtained using a confocal WITec alpha 300 Raman spectrometer.
The spectra were recorded with a 532 nm laser excitation light and
an integration time of 2 s after each preparation step (i.e., air-annealed, nitridated, and TiOxNy–Ir samples) and finally after EC-STAT
analysis. The air-annealed form of the sample was extremely sensitive
to laser light excitation, demanding a low laser power of 0.6 mW and
also a diminished number of scans [from 100 (a) to 20 (b,c) scans
in
corrected (due to fluorescence), while spectra of others are shown,
as measured in insets in
measurements of other samples (nitridated, TiOxNy–Ir and after EC-STAT),
we used a protocol that can serve as a sample stability estimation.
Namely, we measured single Raman spectra sequentially at a certain
site using increasing laser powers of 0.6, 1.4, 3.4, 7.3, and 13.5
mW. Each sample on the TEM grid was examined at 3 sites. At higher
laser powers, the samples suffered degradation, but the extent of
degradation can be taken as a measure for the stability of the sample.
The results are shown in the