名称:
Me3SiCC–CMeCH2 copper(I) β-diketonates: Synthesis, solid state structure, and low-temperature chemical vapour deposition
摘要:
The ene-yne copper(I) beta-diketonates [(eta(2) -TMSMB)Cu(beta-diketonate)] (beta-diketonate = acetylacetonate/acac, 5; = 1,3-di-tertbutylacetonate/dbac, 6;=1,1,1,5,5,5-hexafluoroacetylacetonate/hfac, 7; TMSMB=4-TriMethylSilyl-2-Methyl-But-1-ene-3-yne, Me3SiC=C-CMe=CH2) are accessible by the reaction of [(eta(2) -TMSMB)Cu(mu-Cl)](2) (3) with [Na(beta-diketonate)] (beta-diketonate = acac, 4a; = dbac, 4b; = hfac, 4c) in a 1:2 molar ratio. Complexes 6 and 7 are also formed, when Cu2O (8) is reacted with H-hfac (9a) or H-dbac (9b), respectively.The solid state structure of 7 is reported. The copper(l) ion possesses a planar environment caused by the eta(2)-coordinated TMSMB ligand and the chelate-bound hfac group, while the CMe=CH2 entity stays free.The thermal properties of 5-7 were determined by applying ThermoGravimetry (TG) and Differential Scanning Calorimetry (DSC). All complexes decompose in a two-step process beginning at ca. 85 degrees C. Elimination of TMSMB produces [Cu(beta-diketonate)] which disproportionates to give [Cu(beta-diketonate)2] and elemental copper.Preliminary hot-wall Chemical Vapour Deposition experiments (CVD) were carried out with 7. Copper films were deposited onto TiN-coated oxidised silicon wafers at a precursor vaporisation temperature of 50 degrees C and a deposition temperature of 145 degrees C. The films were characterised by SEM and EDX. (c) 2005 Elsevier B.V. All rights reserved.