Within a combinatorial investigation, a gradient sputtered gold layer on top of polystyrene on silicon substrate is addressed. Results from a real-space inspection by transmission electron microscopy are compared with surface-sensitive microbeam grazing incidence small-angle x-ray scattering. The combinatorial approach allows distinguishing different morphologies prepared under exactly the same environmental conditions on one single substrate. The transition of a coalescent layer to an isolated nanoparticle layer is determined as a function of sputter rate. Though optical spectra show only slight differences, the morphology and structure are distinctly different from evaporated layers prepared with same mass thickness.

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