| Chapter One. An overview of the use of mercury as a solvent for preparing intermetallic and oxide materials is given.; Chapter Two. The intermetallic compounds Al2Au, AlAu, AlAu2, Al3Pd2, and AlPd can be prepared in high yield either as single products or as multiple products by dissolution of the elements in liquid mercury at ∼350°C, followed by distillation of the solvent. A systematic study reveals that the products of these reactions depend strongly on initial mole ratios. Some of the reactions are shown to be kinetically controlled. Direct synthesis reactions tend to be favored for concentration ratios corresponding to intermetallic phases that exhibit a coexistence tie-line with the Hg solution.; Chapter Three. Oxide monoliths of certain active metals (Al, Sc, Y, lanthanides) with the particle size in the nanoscale range can be prepared by dissolving the metal in mercury and subsequently exposing the solution to air. In some cases, single-phase oxide products can be grown from solutions comprising two different metals (SCxY2−xO 3; 0 ≤ x ≤ 2). For some systems, mixed oxides can be prepared by distilling Hg from binary metal solutions and then exposing the resultant metal powder to air (AlSmO3).; Chapter Four. Decomposition chemistry of the four most common CVD precursors for LiNbO3—[Li(OBut)]6, Li(tmhd), [Nb(OEt)5]2 and Nb(tmhd)4 (OBu t = tertiary butoxide, OEt = ethoxide, tmhd = 2,2,6,6-tetramethyl-3,5-heptanedionate)—was examined under high vacuum conditions. The metal β-diketonates are unstable under these conditions. The metal alkoxides, while of greater thermodynamic stability, are subject to autocatalytic processes that inhibit film growth: these processes generate volatile metal-containing moieties that subsequently desorb from the surface.; Chapter Five. The compounds Nb(OEt)4(DMAE) and Nb(OEt)3(DMAE)2 were prepared by exchange reactions between Nb(OEt)5 and HOCH2CH2N(CH3) 2 in 1:1 and 1:2 ratios in benzene solutions at room temperature. Solution behavior of Nb(OEt)4(DMAE) and Nb(OEt)3(DMAE)2 is very complex and depends on a number of parameters, including solvent, concentration, and temperature. While it is fairly certain that Nb(OEt) 4(DMAE) is predominantly monomeric in benzene solutions at low concentration, some indications for dimer formation were obtained at high concentrations. The structure of Nb(OEt)3(DMAE)2 cannot be deduced with the data in hand. |
