Thin films of nickel sulfide (NiS 1.03 , NiS 2 ,a-Ni 7 S 6 , or mixtures thereof) and palladium sulfide (PdS, Pd 16 S 7 , Pd 4 S, or mixtures thereof) have been prepared by aerosol-assisted (AA)CVD using dithiocarbamate precursors of the type M(S 2 CNRR') 2 (M = Ni, Pd; RR' = Et 2 , MeEt, Me n Bu, or Me n Hex). The solid-state structure of Ni(S 2 CNMe n Bu) 2 , was determined by X-ray single-crystal diffraction and is characteristic of known nickel dithiocarbamates. Films were grown on glass substrates at temperatures of 400-525°C and characterized by X-ray diffraction (XRD), energy dispersive analysis of X-rays (EDAX), and scanning electron microscopy (SEM).