The preparation of palladium catalyst particles deposited by ion excha
nge on the activated surface of highly oriented pyrolytic graphite (HO
PG) has been investigated by STM and ESCA methods. Each step of the pr
eparation procedure was characterized in a parallel way using the two
techniques. After oxidation treatment of the graphite substrate chemic
al oxidized functions are revealed by ESCA, while STM images indicate
that both chemical and physical sites are created. Ion exchange of a p
alladium salt solution with the activated carbon surface gives isolate
d particles. It appeared that the preliminary oxidation treatment cond
itions play an important role in the size and surface distribution of
particles. These parameters are further modified by the final hydrogen
reduction treatment which induces a migration of palladium which conc
entrates near physical sites.