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Nanocomposite films consisting of Au and/or Cu nanoclusters embedded in amorphous carbon matrices were characterized by anomalous grazing incidence small-angle X-ray scattering (AGISAXS) using synchrotron radiation. Whenever relative intensities can be measured with precision, it is shown that AGISAXS, being element specific, is a powerful method for separating the scattering contributions of two types of metallic nanoclusters. Two method­ologies to analyse AGISAXS data are compared; the differential method appears the most efficient since it permits separation of the scattering from one type of nanocluster from the other contributions including other types of nanocluster, surface roughness or defects.

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