[Ag{S
<sub>2</sub>
CNR(C
<sub>2</sub>
H
<sub>4</sub>
OH)}] as Single‐Source Precursor for Ag
<sub>2</sub>
S – Synthesis, Decomposition Mechanism, and Deposition Studies
作者:Robert Mothes、Alexander Jakob、Thomas Waechtler、Stefan E. Schulz、Thomas Gessner、Heinrich Lang
DOI:10.1002/ejic.201403182
日期:2015.4
AbstractSilver(I) dithiocarbamates [AgS2CNR(C2H4OH)}] (3a, R = Me; 3b, R = Bu) were accessible by the reaction of AgNO3 with KS2CNR(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.