In this study, four Fe(III) dithiocarbamate complexes were synthesized and characterized by spectro-scopic techniques and thermogravimetric analysis. Thermogravimetric analysis of the complexes showed they decomposed to iron sulphide. The complexes were used as single source precursors and thermolysed in HDA to prepare iron sulphide nanoparticles. The iron sulphide nanoparticles were incorporated into polyvinyl alcohol (PVA) to form iron sulphide/PVA nanocomposites. UV-Vis, PL, FTIR, TEM, EDS and XRD were used to study the optical and structural properties of the nanoparticles and PVA nano composites. The absorption spectra of the nanoparticles are blue shifted with respect to the absorption band edges. The FTIR confirmed the incorporation of the nanoparticles in the PVA matrix by the slight shift of the O-H and C-O bands and the intense peaks on the nanoparticles. Rod-like and spherical shaped particles were observed from the TEM images with crystalline sizes for the nanoparticles in the range 6.49-7.89 nm and 8.17-18.35 nm for the nanocomposites. The XRD showed that the nanoparticles and nanocomposites have a greigite crystalline phase with crystalline size in the range 1.50-1.54 nm for the nanoparticles and 1.64-2.03 nm for the nanocomposites. (C) 2017 Elsevier B.V. All rights reserved.