MoOx/ZrO2 samples (Mo content, 0.7 to 4.0 atoms nm-2) have been invest
igated by XPS and Fourier transform Infrared (FTIR) spectroscopies. Af
ter heating in O2 (773 K), XPS shows the presence of Mo(VI) species; w
hile the IR analysis shows bands in the 830-1012 cm-1 region, arising
from Mo(VI) species of various nuclearity. In the early stages of the
reduction (H-2 at 500 K) both XPS and IR show the formation of Mo(V).
In agreement with previous ESR results, the intensity of IR and XPS ba
nds from Mo(V) does not appreciably change by further increasing the e
xtent of reduction up to 803 K. On extensively reduced samples, both I
R and XPS show the presence of Mo(IV) in addition to Mo(VI) and Mo(V).
Upon NO adsorption at RT, dinitrosyls of Mo(IV) were detected by IR.
A further rise in the extent of reduction with H-2 at 803 K, led to a
drop in the intensity of the IR band from Mo(IV) and XPS detected Mo m
etal.