The work described here involves a detail AACVD study to observe and investigate overall morphological changes in copper, silver and nickel sulphide depositions from respective dithiocarbamate complexes on zinc oxide, bismuth and silver functionalized thin films at three different temperatures i.e. 300, 350, 400 оC. A variation in film thickness and color from black, brown, yellow and shiny dark grey was observed in copper, silver, nickel sulphide on all coated thin films. SEM images clearly indicated variations in morphology and different phases by XRD were observed with different UV analyzed nanoparticle coatings on substrate surface. In addition to above study, another scheme involving detailed investigation on effect of ligand substitution on metal sulphide depositions by synthesis and characterization of a set of N,N-disubstituted-N’-acylthiourea was done. Benzoyl and cinnamoyl chloride, and two secondary amines, diphenyl- and diisopropylamine were selectively used to derive L1, L2, L3, L4 ligands of completely characterized nickel complexes, Ni(L3)2 was found to have the lowest decomposition temperature and its thorough study revealed the most rapid mass loss occurring at 223 °C. L3 was selected for the synthesis and study of several other ML2 and ML3 complexes (M = Ni, Zn, Cd, Fe, Co, and Cu.) depending upon this detail study. The related complexes Ni(L3)2, Cu(L3)2, Co(L3)3, and Zn(L3)2 were all synthesized and found to crystalize in the cis-square planar, trans-square planar, fac-octahedral, and distorted tetrahedral geometries respectively. From AACVD, Ni(L3)2, Co(L3)3, and Zn(L3)2 at temperatures of 350 °C were found to deposit their corresponding metal sulfide but attempted depositions from tetrahydrofuran solution of Cu(L3)2 were not very successful due its low solubility. The viability of N,N-disubstituted-N’-acylthiourea ligands as sulfur sources in the AACVD of metal sulfides was demonstrated in these experiments.