Raman spectroscopy, FTIR and scanning tunneling microscopy (STM) were used to study diamond-like nanocomposite (DLN) and metal containing DLN (Me-DLN) films. The FTIR spectra showed no appreciable absorption from the C-H stretch vibration band in DLN when 1 kV rf bias voltage was applied. Thermal annealing (450°C for 2 hrs) of (a) DLN and Cr-DLN films caused no change in the Raman spectra while (b) for Pt-DLN films there was a blue shift of both the crystalline (G) and microcrystalline (D) graphite-like features, an increase in the ID/IG intensity ratio and a decrease in the linewidths. The changes observed were more pronounced in the film with the highest Pt concentration. The STM image of this Pt-DLN film revealed a structure of aromatic graphite rings.