*3.2. Catalyst Characterization*

X ray di ffraction analyses were carried out using a PW1050/81 di ffractometer (Philips/Malvern, Royston, UK) equipped with a graphite monochromator in the di ffracted beam and controlled by a PW1710 unit (Cu K α, λ = 0.15418 nm). A 2θ range from 20◦ to 80◦ was investigated at a scanning speed of 40◦/h. Nitrogen adsorption-desorption isotherms were determined at liquid nitrogen temperature (−196 ◦C), using an automatic ASAP 2020 absorptiometer (Micromeritics, Norcross, GA, USA) and analyzed using a software operating standard Brunauer–Emmett–Teller (BET) and BJH methods. Raman analysis was carried out with a micro-spectrometer Raman RM1000 (Renishaw/Thermo Fisher, New Mills, Wotton-under-Edge, Gloucestershire, UK) interfaced to a microscope Leica DMLM (objective 5×, 20×. 50×). The available sources were an Ar<sup>+</sup> laser (λ = 514.5 nm; Pout = 25 mW) and a diode laser (λ = 780.0 nm; Pout = 30mW). In order to eliminate the Rayleigh scattering, the system was equipped with a notch filter for the Ar<sup>+</sup> laser and an edge filter for the diode one. The network was a monochromator with a pass of 1200 lines/mm. The detector was a CCD one (Charge-Coupled Device) with a thermo-electrical cooling (203 K). TEM analyses were carried out using a TEM/STEM TECNAI F20 microscope (FEI, Hillsboro, OR, USA) combined with Energy Dispersive X-Ray Spectrometry (EDS), at 200 keV. The sample preparation was carried out by suspending the powder in ethanol and treating it with ultrasound for 15 min. The suspension was deposited on a "multifoil-carbon film" sustained by a Cu grid. Then the so-prepared system was dried at 100 ◦C.
