Synthesis And Characterization Of Organophosphate Stabilized Copper(I)/Silver(I) Complexes; Synthesis And Purification Of Silicon/Iron Containing Single Precursor

This thesis includes the following two parts. Part one: A series of Lewis-base stabilized copper(I) and silver(I) complexes were synthesized. The complexes obtained were characterized by IR, 1H NMR, 13C{H} NMR and elemental analysis. Some of the complexes were also determined by X-ray single crystal analysis. Part two: (SiCl3)2Fe(CO)4 was synthesized by using Fe(CO)5 as starting material via several steps, which could be used as the precursor for growingβ-FeSi2 film by chemical vapor deposition techniques. The purification method was studied and the purity of the final product was measured by ICP-MS.Part one: Synthesis and Characterization of organophosphine/phosphite stabilized copper(I) complexes.A series of organophosphine/phosphite stabilized copper(I) methanesulfonates of type [LnCuO3SCH3] (L = Ph3P, n = 1, 2a; n = 2, 2b; n = 3, 2c; L = (EtO)3P; n = 1, 2d; n = 2, 2e; n = 3, 2f) were synthesized by using CH3SO3Ag, CuCl and organophosphine/phosphate [Ph3P/(EtO)3P] as starting material. Complexes obtained have been characterized by elemental analysis, 1H NMR, 13C{H} NMR and IR spectroscopy, respectively.Part two: Synthesis and Characterization of Organophosphine/phosphite Stabilized Silver(I) Complexes.A series of organophosphine/phosphite stabilized silver(I) methanesulfonates of type [LnAgO3SCH3] (L = Ph3P, n = 1, 3a; n = 2, 3b; n = 3, 3c; L = (EtO)3P; n = 1, 3d; n = 2, 3e; n = 3, 3f) were synthesized by using CH3SO3Ag and organophosphine/phosphate [Ph3P/(EtO)3P] as starting material. Complexes obtained were characterized by elemental analysis, 1H NMR, 13C{H} NMR and IR spectroscopy, respectively. The molecular structures of complexes 3a and 3b have been determined by X-ray single crystal analysis. The crystal structure reveals that complex 3a exists as a tetramer [Ph3PAgO3SCH3]4 in "cubane-like" frameworks, and complex 3b exists as a monomer in crystal structure. Part three: Synthesis and Purification of Silicon/Iron Single Precursor.(SiCl3)2Fe(CO)4 was synthesized by using HSiCl3 reacting with Fe3(CO)12 under high pressure and high temperature. The product obtained was characterized by, infrared spectroscopy (IR) and X-ray single crystal analysis, respectively. The crystal structure reveals that each molecule contains one Fe atom, four carbonyls and two -SiCl3 groups, which means in each molecule the proportion of Fe atom and Si atoms is 1: 2. The purification method was studied and the compound purified was measured by using ICP-MS. ICP result shows that product purity reaches 99.976%. This compound is a good precursor for growingβ-FeSi2 by MOCVD techniques.