The
reducibility of iron oxide nanoparticles (NPs) supported over
few-layer thick graphite upon annealing in hydrogen is investigated
by near ambient pressure X-ray photoelectron spectroscopy (NAP-XPS),
X-ray absorption spectroscopy (XAS), electron energy loss spectroscopy
(EELS), and high-resolution transmission electron microscopy (HR-TEM).
It is found that the stability of the iron oxide NPs toward reduction
is enhanced by the interaction with the graphene nanosheets as compared
to the bulk iron oxide. Postannealing TEM micrographs reveal the existence
of both core/shell and homogeneous iron oxide NPs with the latter
forming irregular trenches into the graphene sheets. EELS analysis
and TEM images clearly demonstrate that the reducibility of iron oxide
particles depends on the specific graphene site on which they are
attached. Furthermore, we show that graphene etching can be mediated
by iron oxide NPs at relatively mild reduction conditions.