三正丁基膦稳定的铜(Ⅰ)β-二酮配合物的合成、表征以及作为前驱物用化学汽相沉积法生长铜膜

摘要

A series of copper(Ⅰ)β-diketonate complexes of type [(nBu3P)mCuL] [m=1 or 2. m=1: L=acac (4), acac=acety lacetonate; L=dbac (5), dbac=1,3-di-tert-butylacetonate; L=hfac (6), hfac=1, 1, 1, 5, 5, 5-hexafluoroacetylaceto nate; m=2: L=acac (7); L=dbac (8); L=hfac (9)] with nBu3P as ancillary Lewis-base ligand is accessible by the reaction of [(nBu3P)mCuCl] (1: m=1, 2: m=2) with the sodium-β-diketonate salts NaL (3a: L=acac; 3b: L=dbac; 3c:L=hfac) in a 1:1 molar ratio. Complexes 7～9 can also be prepared by treatment of 4～6 with one equivalent of rnnBu3P (10).Spectroscopic data (IR,1H-,13C{1H}-NMR)of 4～9 reveal that the respective β-diketonates are chelate -bound to copper(Ⅰ), thus resulting in a tri-(4～6) or trtra-coordination (7～9) at the transition metal ion.The thermal properties of 4～9 were studied by ThermoGravimetric anlaysis (TG) and Differential Scanning Calorometry (DSC).Hot -wall Chemical Vapour Deposition experiments (CVD) were carried-out by using ,for example ,complexes 4 and 7 as precursors for the deposition of copper onto TiN-coated SiO2 wafers. SEM and EDX studies were applied to characterize the obained copper films.%合成了一系列三正丁基膦辅助配体稳定的铜(Ⅰ)β-二酮配合物,对合成的配合物用元素分析、红外、核磁共振以及热重和差热等手段进行了表征.筛选出性能优良的配合物为前驱物用化学汽相沉积(CVD)的方法生长出金属铜膜,用SEM和EDX等手段对生长的铜膜进行了表征.