Characterization of surface Ag nanoparticles in nanocomposite a-C:Ag coatings by grazing incidence X-ray diffraction at sub-critical angles of incidence

Silver diffusion within nanocomposite films and/or toward the film surface is often observed during annealing of the silver-based nanocomposite films. In order to control and/or minimize this process, it is crucial to characterize the aggregated silver nanoparticles on the films surface. In this paper grazing incidence X-ray diffraction (GIXRD) with both sub-critical and supra-critical angles of incidence is used to characterize the Ag nanoparticles distribution, shape and structure both inside the matrix and on the nanocomposite film surface. The nanocomposite carbon coating containing Ag nanoparticles (a-C:Ag) was deposited by dc magnetron sputtering. The coatings were analyzed by GIXRD using fixed incident angles both below and above the critical angle for total reflection. By using sub-critical angles it was possible to eliminate diffraction from the bulk material allowing to estimate the size distribution of the nanoparticles sitting on the surface. The results obtained by GIXRD analysis were checked through comparison with the observations made by both TEM and SEM analysis. The proposed methodology can be used to characterized nanoparticles deposition on a surface and/or island formation during film growth as long an adequate substrate with high critical angle for total reflection is used. (orig.)