Powdery Pd/graphite model catalysts were studied with transmission electron microscopy (TEM), scanning
tunneling microscopy (STM), and scanning tunneling spectroscopy (STS), with the later two techniques
in air. In contrast to TEM images, STM/STS data are representative of the very surface and are therefore
more relevant for an interpretation of the catalytic properties of these kind of catalysts. Besides spherical
clusters and layered structures, also platelike and diffuse structures could be distinguished in the STM
images. An assignment of the different objects to one of the main elementsgraphite and palladiumwas
possible with STS. The I(V) curves on graphite are always much narrower on the V axis than those on
palladium, and their slope dI/dV is, thus, larger. Utilizing this distinction, “chemical maps” were determined
by taking I(V) data over a grid of surface points and assigning each point the value of the integral under
its dI/dV curve. The comparison of such a chemical map with the topographic STM picture of the same
area shows that only the spherical cluster structures consist of palladium, in accordance with the TEM
pictures. The layered and platelike structures are identified as graphite, and the diffuse structures probably
belong to impurities. In any case, the latter consist neither of graphite nor of palladium. A statistical
analysis of the cluster morphology reveals that at low Pd loads the clusters are of spherical shape whereas
the average width-to-height ratio increases at higher concentrations. The clusters at higher Pd concentrations
exhibit a more elliptical shape.