Abstract
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.
Highlights
Iron sulfide, the most abundant transition metal chalcogenide in the earth’s crust, is potentially significant for several applications including biomedical and catalytic processes,[1,2] hydrogen generation,[3,4] environmental remediation,[5] batteries and solar cells.[6,7,8] Potentially, it has a number of advantages over many other materials including low toxicity and cost, vacancydependent crystalline structures which could be useful in bandgap tuning across quantum confinement regimes, as well as interesting magnetic and electric properties.[9]
Structural refinement data are given in the Experimental section; selected bond angles and lengths are presented in the caption to Fig. 1(a)
We have successfully synthesized tris-( piperidinedithiocarbamato)iron(III) (1) and tris-(tetrahydroquinolinedithiocarbamato)iron(III) (2) complexes and determined their X-ray crystal structures. Both complexes have been used as single source precursors for the deposition of iron sulfide thin films on glass substrates by the aerosol assisted chemical vapor deposition technique
Summary
The most abundant transition metal chalcogenide in the earth’s crust, is potentially significant for several applications including biomedical and catalytic processes,[1,2] hydrogen generation,[3,4] environmental remediation,[5] batteries and solar cells.[6,7,8] Potentially, it has a number of advantages over many other materials including low toxicity and cost, vacancydependent crystalline structures which could be useful in bandgap tuning across quantum confinement regimes, as well as interesting magnetic and electric properties.[9]. These complexes have been used as single-source precursors for the deposition of iron sulfide thin films by AACVD. Powder X-ray diffraction, scanning electron microscopy and optical measurements reveal that the structural and electronic properties of the as-prepared nanostructured iron sulfide films are strongly dependent on sample preparation conditions such as temperature and solvent effects.
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