Phosphane- and phosphite-silver(I) phenolates: Synthesis, characterization and their use as CVD precursors
作者:Alexander Jakob、Heike Schmidt、Bernhard Walfort、Tobias Rüffer、Thomas Haase、Katharina Kohse-Höinghaus、Heinrich Lang
DOI:10.1016/j.ica.2010.05.049
日期:2011.1
The silver(I) salts [AgOR] (3a, R = C9H6N; 3b, R = C6H4-2-CHO, 3c, R = C6H4-2-Cl; 3d, R = C6H4-2-C N; 3e, R = C6H4-2-NO2) are accessible by the stoichiometric reaction of [AgNO3] (1) with HOR (2a, R = C9H6N; 2b, R = C6H4-2-CHO; 2c, R = C6H4-2-Cl; 2d, R = C6H4-2-C N; 2e, R = C6H4-2-NO2) in presence of NEt3. Treatment of 3a-3e with (PBu3)-Bu-n (4), P(OMe)(3) (5a) or P(OCH2CF3)(3) (5b) in the ratios of 1:1 and 1:2, respectively, produced complexes [LmAgOR] (L = (PBu3)-Bu-n, m = 1: 6a, R = C9H6N; 6b, R = C6H4-2-CHO; 6c, R = C6H4-2-Cl; 6d, R= C6H4-2-C N; 6e, R= C6H4-2-NO2. m = 2: 7a, R= C9H4; 7b, R= C6H4-2-CHO; 7c, R= C6H4-2-Cl; 7d, R = C6H4-2-C N; 7e, R = C6H4-2-NO2. L = P(OMe)(3), m = 1: 8a, R = C6H4-2-CHO; 8b, R = C6H4-2-NO2. m = 2: 9, R = C6H4-2-NO2. L = P(OCH2CF3)(3), m = 1: 10, R = C6H4-2-NO2). Based on TGA, temperature-programmed and in situ molecular beam mass spectrometry metal-organic 7e was applied as CVD precursor in the deposition of silver onto glass substrates. The resulting silver films were characterized by XRD. The SEM image of a film grown from 7e at 350 degrees C showed a homogeneous surface with grain sizes of 40 nm. The molecular structures of 8b and 10 in the solid state were determined. They are isostructural and are cubane-like structured. Low-temperature P-31H-1} NMR studies showed that the title complexes are dynamic in solution and exchange at room temperature their ligands. (C) 2010 Published by Elsevier B.V.