The surface composition of Pt25Ni75(111) has been determined by ion sc
attering spectroscopy and Auger electron spectroscopy. The surface lay
ers are found to be enriched in Pt due to preferential sputtering. The
rmal treatment induces further segregation of Pt at the topmost atomic
layer. From the different sampling depths of ISS and AES composition
profiles are deduced, which show a strong dependence on the temperatur
e during thermal treatment. At an annealing temperature of 770 K the t
hermally induced Pt segregation is determined by the composition of th
e sputter induced altered layer being enriched in Pt. However, at an a
nnealing temperature of 970 K the sputter induced altered layer has di
sappeared and the Pt segregation at the topmost atomic layer is determ
ined by the bulk composition.