New hybrid magnetic materials based on HDPE filled with Со and Ni nanoparticles have been prepared via the metal vapor synthesis. Properties of the metal-polymer composites have been elucidated as a function of MVS parameters and metal nature. The Faraday method has been applied to characterize the magnetic properties of the systems. The microstructure of the samples has been studied with a number of X-ray and synchrotron techniques, including XRD, EXAFS and SAXS. Core-level and valence band spectra were measured by XPS. The peak at binding energy of 282.8 eV characteristic of C-Ni bond was recorded in the C 1s spectrum. It was shown that properties of nanocomposite materials with similar compositions are determined both by the synthesis conditions and post-synthesis factors.