M. Tech. (Department of Chemistry, Faculty of Applied and Computer Sciences), Vaal University of Technology. / In chemical bath deposition (CBD) method, deposition of metal chalcogenide semiconducting thin films occurs due to substrate maintained in contact with a dilute chemical bath containing metal and chalcogenide ions. Semiconducting nickel sulphide (NiS) and iron sulphide (FeS) thin films have been prepared on a glass substrate by varying the deposition parameters such as the concentration of solutions, deposition time, temperature and pH. Multi-layered thin films were deposited on glass substrate and the spin-cast conductive polymer, poly (3.4-ethylenedioxythiopene) polystyrene sulfonate (PEDOT: PSS) was intercalated. The characterization of the films was carried out using UV-Vis spectroscopy, scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDX), atomic force microscopy (AFM) and X-ray diffraction (XRD). Single layer nickel sulphide was deposited at room temperature, pH 10 and the deposition period of 3 hours, triethanolamine was used as the complexing agent. Iron sulphide was deposited for 6 hours at 70 °C with the pH of 2.5 using EDTA as a complexing agent. Generally the iron and nickel sulphide were prepared from their respective nickel or iron salt and the thiourea or thiosulfate as a source of sulphide ions in solution. SEM and AFM results show that the FeS film is evenly coated and has uniform grain size with the roughness of ~22.4 nm and thickness of ~23.8 nm. The optical absorption analysis of FeS showed the band gap energy of ~2.9 eV which blue shifted from the bulk. The EDX analysis confirms the compositions of iron and sulphur in FeS films. XRD pattern showed amorphous films for both FeS and NiS thin films due to the amorphous nature of the glass substrate. The optical data of NiS film were analysed and exhibited the band gap energy of ~3.5 eV and ~3.3 eV for successive ionic layer adsorption and reaction (SILAR), which is the modified CBD, both blue shifted from the bulk. The films were observed to have thickness value of ~35.7 nm and ~2.3 nm SILAR with the roughness of ~112.5 nm and ~35.4 nm SILAR from AFM results. SEM confirmed the uniformly distributed film presented by AFM analysis. The chemical composition of Ni and S were confirmed by EDX spectra. The PEDOT: PSS was intercalated between the FeS as the first layer and NiS as the top layer which gave the thickness of ~18.7 nm and roughness of ~115.2 nm from AFM analysis. PEDOT: PSS acted as a passive layer that protects and stabilize the FeS layer and NiS as the third active layer which enhanced the optical absorption of the film when using SILAR method for solar application.