Accession Number : ADA318405
Title : Formation, Structural Characterization, and Thermal Decomposition of the Adducts, X3Ga*P(TMS)3?X=C1,Br,I!.
Descriptive Note : Technical rept.,
Corporate Author : DUKE UNIV DURHAM NC DEPT OF CHEMISTRY
Personal Author(s) : Janik, Jerzy F. ; Baldwin, Ryan A. ; Wells, Richard L. ; Pennington, William T. ; Schimek, George L.
PDF Url : ADA318405
Report Date : 30 OCT 1996
Pagination or Media Count : 24
Abstract : The adducts, X3Ga-P(TMS)3 X = C1 (1), Br (2), 1(3), were prepared in high yields from the combination of the respective gallium trihalides with P(TMS)3 in hydrocarbon solvents at ambient temperature. The adducts were characterized by NMR, MS, elemental analysis, and single-crystal X-ray stmcture determinations. Particularly, the 1H NMR study of 1-3 helped correct our previously published results regarding momomer-dimer equilibria of the related X2GaP(SiMe3)22 in solution. The crystal structure determinations showed that 1 and 2 were solvated, 1-C6H5Cl and 2-C7H8, respectively, and that 3 was solvent-free. The thermal decomposition behavior of 1-3 was studied by TGA along with a determination of the volatiles from pyrolysis and analysis of the final solid product. The pyrolyses of 1-3 at 450 deg C under vacuum resulted in nanocrystalline GaP with 4-5 nm particle average sizes as determined by X-ray powder diffraction (XRD) and, for pyrolysis of 2, by transmission electron microscopy (TEM); in addition, small quantities of amorphous S/C/H containing phases were also formed.
Descriptors : *THERMAL PROPERTIES, *X RAY DIFFRACTION, *CRYSTALLIZATION, *HYDROCARBONS, TEMPERATURE, NUCLEAR MAGNETIC RESONANCE, QUANTITY, POWDERS, VACUUM, AMORPHOUS MATERIALS, SOLIDS, ELECTRON MICROSCOPY, TRANSMITTANCE, PARTICLES, YIELD, GALLIUM, SOLVENTS, VOLATILITY, DETERMINATION, PYROLYSIS.
Subject Categories : Radiobiology
Distribution Statement : APPROVED FOR PUBLIC RELEASE