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[Ag{S2CNR(C2H4OH)}] as single-source precursor for Ag2S – synthesis, decomposition mechanism, and deposition studies

: Mothes, R.; Jakob, A.; Waechtler, T.; Schulz, S.E.; Gessner, T.; Lang, H.


European journal of inorganic chemistry 2015 (2015), Nr.10, S.1726–1733
ISSN: 1434-1948
ISSN: 1099-0682
Fraunhofer ENAS ()

Silver(I) dithiocarbamates [Ag{S2CNR(C2H4OH)}] (3a, R = Me; 3b, R = Bu) were accessible by the reaction of AgNO3 with K{S2CNR(C2H4OH)} (2a, R = Me; 2b, R = Bu). Alternatively, 3b could be prepared by the condensation of CS2 and Ag2O with NHBu(C2H4OH) (1b). The thermal behavior of 3 was studied by thermogravimetric (TG) analysis. A two-step decomposition process leads to the formation of α-Ag2S, as evidenced by X-ray powder diffraction studies. A decomposition mechanism of 3a to form Ag2S through the release of 3-methyloxazolidine-2-thione is discussed based on TG–MS, GC–MS, and NMR experiments. Because of the better solubility of 3b, this complex was tested for Ag2S spin-coating deposition studies on different substrates (SiO2/Si, TiN/SiO2/Si, glass) with subsequent annealing at 450 °C under a N2 atmosphere. Film thickness, composition, and morphology of the as-deposited films were determined by XRD, SEM, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy, which showed the formation of 200 nm thick, conformal, adherent, monoclinic α-Ag2S layers.