The synthesis and single-crystal X-ray structure of bis(piperidinedithiocarbamato)pyridinecadmium(II), [Cd(S2C(NC5H10))2(NC5H5)] are reported and its use as a precursor for the synthesis of hexagonal CdS nanoparticles and CdS thin films is presented. Thermogravimetric analysis (TGA) of this complex showed clean decomposition in two steps to give CdS. Thermolysis of the complex in hexadecylamine at different temperatures in the range 190–270 °C gave CdS nanostructures including nanorods and oval shaped particles. The band gap of the as-synthesized CdS nanoparticles varied as the temperature was increased. CdS thin films with optical direct band gaps of ca. 2.4 eV were deposited by aerosol-assisted chemical vapour deposition (AACVD) in the temperature range 350 to 450 °C using the same precursor. Powder X-ray diffraction (p-XRD) patterns of CdS nanoparticles and thin films confirmed the hexagonal phase of CdS.
Tris-(piperidinedithiocarbamato)iron(III) (1) and tris-(tetrahydroquinolinedithiocarbamato)iron(III) (2) complexes have been synthesized and their single-crystal X-ray structures were determined. Thermogravimetric analysis (TGA) of the complexes showed decomposition to iron sulfide. Both complexes were then used as single-source precursors for the deposition of iron sulfide thin films by aerosol-assisted chemical vapour deposition (AACVD). Energy-dispersive X-ray (EDX) spectroscopy confirmed the formation of iron sulfide films. The addition of tert-butyl thiol almost doubled the sulfur content in the deposited films. Scanning electron microscopy (SEM) images of the iron sulfide films from both complexes showed flakes/leaves/sheets, spherical granules and nanofibres. The sizes and shapes of these crystallites depended on the nature of the precursor, temperature, solvent and the amount of tert-butyl thiol used. The observed optical properties are dependent upon the variation of reaction parameters such as temperature and solvent. Powder X-ray diffraction (p-XRD) studies revealed that pyrrhotite, hexagonal (Fe0.975S), marcasite and smythite (Fe3S4) phases were differently deposited.