Formation, Structural Characterization, and Thermal Decomposition of the Adducts, X3Ga*P(TMS)3?X=C1,Br,I!.
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.
Document Details
- Document Type
- Technical Report
- Publication Date
- Oct 30, 1996
- Accession Number
- ADA318405
Entities
People
- George L. Schimek
- Jerzy F. Janik
- Richard L. Wells
- Ryan A. Baldwin
- William T. Pennington
Organizations
- Duke University