| Recent research in our laboratory has centered around the synthesis and characterization of organometallic compounds containing bonds between atoms of group 13 and group 15. Primarily, reactions between metal halides and silyl pnicogens have been utilized to form these compounds, with the concomitant elimination of silyl halide, i.e. dehalosilylation. The impetus for this research lies in the production of single-source precursors to semiconductor materials, and extends into the burgeoning field of nanocrystal technology, based on the phenomenon known as "quantum confinement".; The work presented herein extends classical synthetic techniques into the Ga-P system. Through the use of dehalosilylation, new compounds have been synthesized which contain the Ga-P bond. These include two Lewis acid/base adducts containing phenyl groups on the gallium centers, and a novel compound which exhibits mixed-bridging of two gallium centers by a chlorine atom and a phosphorus atom. In addition, a new class of dimeric species has been isolated and characterized by X-Ray crystallography. These dimers contain all exocyclic halogen ligands on the metal centers, and are the first of this type reported in the Ga-P system.; Several of the novel compounds isolated have been thermally decomposed to yield powders containing nanocrystalline GaP. This thermolysis has been studied by thermogravimetric analysis (TGA). The powders have been characterized by elemental analysis and X-Ray powder diffraction (XRD). Analysis of the XRD powder patterns of the GaP resulting from each of the precursors indicates a mean particle size of ca. 3 nm. In addition, a new precursor to GaP of the formula ({dollar}rm Gasb2PClsb3)sb{lcub}n{rcub}{dollar} has been prepared and thermolyzed. A similar precursor of the formula ({dollar}rm Gasb2(P/As)Clsb3rbrack sb{lcub}n{rcub}{dollar} has also been studied. The thermolysis product of this material has been characterized by elemental analysis, XRD and X-Ray photoelectron spectroscopy (XPS). Through the analysis, we conclude that the material consists of a solid-solution of GaP and GaAs of the empirical formula {dollar}rm GaAssb{lcub}x{rcub}Psb{lcub}y{rcub}{dollar} (0.6 {dollar}<{dollar} x,y {dollar}<{dollar} 0.9). This represents one of the first reported solid-state syntheses of a ternary 13-15 material. |
