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[Ag{S 2 CNR(C 2 H 4 OH)}] as Single‐Source Precursor for Ag 2 S – Synthesis, Decomposition Mechanism, and Deposition Studies
Author(s) -
Mothes Robert,
Jakob Alexander,
Waechtler Thomas,
Schulz Stefan E.,
Gessner Thomas,
Lang Heinrich
Publication year - 2015
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201403182
Subject(s) - chemistry , x ray photoelectron spectroscopy , monoclinic crystal system , thermal decomposition , tin , thermogravimetric analysis , crystallography , x ray crystallography , analytical chemistry (journal) , diffraction , crystal structure , chemical engineering , organic chemistry , physics , engineering , optics
Silver(I) dithiocarbamates [Ag{S 2 CNR(C 2 H 4 OH)}] ( 3a , R = Me; 3b , R = Bu) were accessible by the reaction of AgNO 3 with K{S 2 CNR(C 2 H 4 OH)} ( 2a , R = Me; 2b , R = Bu). Alternatively, 3b could be prepared by the condensation of CS 2 and Ag 2 O with NHBu(C 2 H 4 OH) ( 1b ). The thermal behavior of 3 was studied by thermogravimetric (TG) analysis. A two‐step decomposition process leads to the formation of α‐Ag 2 S, as evidenced by X‐ray powder diffraction studies. A decomposition mechanism of 3a to form Ag 2 S 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 Ag 2 S spin‐coating deposition studies on different substrates (SiO 2 /Si, TiN/SiO 2 /Si, glass) with subsequent annealing at 450 °C under a N 2 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‐Ag 2 S layers.