electron microscopy
was performed with a Sigma 500 Gemini (Zeiss) at 4 kV using an InLens
detector. Energy-dispersive X-ray spectroscopy analysis was performed
using a Bruker Quantax EDS. X-ray photoelectron spectroscopy (XPS)
measurements were carried out on a custom-build spectrometer (Moses)
equipped with an X-ray source from Al Ka radiation (1486.6 eV) and
a hemispherical electron analyzer in the analysis chambers, under
ultra-high vacuum with the base pressure being lower than 1 ×
10–9 mbar. To minimize any beam damage on the sample,
a large probe area of 1 × 10 mm2 and a low X-ray powder
of 30 W were employed. All measurement was done at room temperature
with a 45° emission angle. The binding energy was calibrated
based on the position of the Au 4f7/2 peak (84.0 eV) and
the Fermi level (0 eV).