LIQUID-PHASE METAL VAPOR CHEMISTRY - ROTARY REACTORS AND ELECTRON-BEAM EVAPORATION SOURCES

A new rotatable metal atom reactor that allows electron-beam vaporizations of refractory materials into liquid solutions at reduced temperatures is described. This innovation demonstrably broadens the scope of synthesis from metal atoms and molecular high-temperature species. Details of the instrument and its operation are provided, together with results of studies of charged particle emissions, a description of techniques for quantifying the rate of metal atom deposition, and a description of a variable-temperature transfer tube for removing thermally labile compounds. A simple addition of the furnace that substantially reduces the power required to evaporate even the most refractory elements leads to dramatically increased vaporization rates for modestly powered 2-kW guns. The paper concludes with some test applications of the device in the liquid-phase electron-beam synthesis of some bis(η6-arene) complexes of titanium, vanadium, and molybdenum. © 1990, American Chemical Society. All rights reserved.