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Maynard-Casely, Helen
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article
Soluble Xanthate Compounds for the Solution Deposition of Metal Sulfide Thin Films
Abstract
A series of soluble metal ethylxanthate compounds were synthesised as precursors for metal sulfide thin films to be deposited using solution-based techniques. Initially, a range of soluble, air and moisture stable, organic ethylxanthate (EtXn) salts were synthesised (cation = Me4N (1), Et4N (2), Pr4N (3), Ph4P (4), guanidinium (5), NMeH3 (6), NMe2H2 (7), NMe3H (8), NH4 (9)). Thermogravimetric analysis (TGA) was used to examine their decomposition profiles, which in turn informed the decision of which counter cation is best suited for inclusion in the metal xanthate compounds. Periodic NMR studies and single crystal X-ray diffraction (SXRD) were used to determine the role protic ammonium counter cations play in the detrimental conversion of xanthates to dithiocarbamate anions. The organic salts 1 and 4 were used to form the metal ethylxanthate compounds (Me4N)[M(EtXn)x] (x = 3 for M = Cd (10Cd), Ni (10Ni), Zn (10Zn)); x = 4 for M = La (11La)) and (Ph4P)[M(EtXn)3] (M = Cd (12Cd), Ni (12Ni), Zn (12Zn)). Solubility studies on these compounds were performed using a range of solvents to demonstrate the viability of using these compounds for solution based deposition methods for thin film formation. TGA of the metal xanthate compounds was used to examine their thermal decomposition profiles and the product resulting from thermolysis, which was found to be the respective metal sulfide. In addition, the co-products of thermal decomposition were analysed by headspace gas-chromatography mass-spectrometry (GC-MS) in order to probe the decomposition mechanism of the precursors. In situ variable temperature synchrotron XRD studies on both bulk and thin film samples of 10Cd and 12Cd were used to examine metal sulfide crystalline phase formation. Decomposition of both precursors was found to give CdS in a hexagonal phase, with the addition of CdCl2 found to aid in increasing the crystallite size during crystallisation.