Ni0.35Ag0.65 thin films were studied by means of both x-ray absorption spec
troscopy and x-ray diffraction, in the as-deposited and annealed states. Sh
ort-range-order investigation has established that nickel atoms are either
clustered in small pure Ni aggregates or dispersed in an Ag-rich solid solu
tion. For the as-deposited and 250 degrees C annealed samples, an accurate
interpretation of the diffraction spectra requires one to take into account
a degree of structural coherence between these two phases, which are prefe
rentially oriented with the dense planes parallel to the surface. Local ord
er and long-range-order characterizations then give coherent results. The m
ean size of the pure Ni aggregates increases from approximately 1 nm in the
as-deposited state to 3-5 nm after a 400 degrees C anneal. The maximum Ni
solubility in the Ag matrix was estimated to be around 7 at.% for these sam
ples. All of the reported results-the natures of the various phases, and me
an sizes, shapes and orientations of the aggregates-are discussed with rega
rd to the other structural (extended x-ray absorption fine-structure, anoma
lous small-angle x-ray scattering) and magnetic information.