The ability to produce transition-metal clusters dispersed in a polymeric matrix by metal sputtering and plasma polymerization in a rf capacitively coupled diode reactor svstem was investigated. An in situ plasma diagnostic technique, i.e., optical emission spectroscopy, was used to predict the metal concentration of the film. Characterization of metal-containing plasma-polymerized propane thin films was realized using x-ray photoelectron spectroscopy, x-ray fluorescence, Raman spectroscopy, transmission electron microscopy, and electron diffraction. Evidence is given that the metal is present in its metallic state in the organic matrix and in the form of uniformly dispersed small particles. The shape and size of gold and cobalt particles at equivalent volume fractions are shown to be different, which is reflected in different electrical percolation threshold values for the two systems.