AbstractGrazing incidence small-angle x-ray scattering (GISAXS) allows to investigate precisely the microstructure of nanocomposite thin films containing metal nanocrystals produced using different synthesis techniques. We present results on the size, size distribution, shape, and correlation length of metallic nanoparticles embedded in different matrices fabricated by sequential pulsed laser deposition, magnetron sputtering, and ion-beam sputtering co-deposition. The morphology of the nanoparticles is discussed in terms of the different growth process that takes place in each case.