SYNTHESIS OF NANOCRYSTALLINE INDIUM ARSENIDE AND INDIUM-PHOSPHIDE FROM INDIUM(III) HALIDES AND TRIS(TRIMETHYLSILYL)PNICOGENS - SYNTHESIS, CHARACTERIZATION, AND DECOMPOSITION BEHAVIOR OF I3IN-CENTER-DOT-P(SIME(3))(3)

Nanocrystalline indium arsenide and indium phosphide were synthesized by heating the products of the independent 1:1 mole ratio reactions of InX(3) (X = Cl, Br, I) with As(SiMe(3))(3) and P(SiMe(3))(3), respectively, and the 2:1 mole ratio reaction of InCl3 with As(SiMe(3))(3). The 1:1 mole ratio reaction of As(SiMe(3))(3) with InCl3 produced a black powder, which after annealing at 400 degrees C afforded InAs crystallites of up to 99.96% purity with an average domain size of 9 nm. InAs obtained from the separate 1:1 mole ratio reactions of InBr3 and InI3 with As(SiMe(3))(3) and the 2:1 mole ratio reaction of InCl3 with As(SiMe(3))(3) consisted of crystallites with average domain sizes of 10, 12, and 16 nm, and purities of 99.65%, 85.95%, and 87.90%, respectively. The independent 1:1 mole ratio reactions of InCl3 and InBr3 with P(SiMe(3))(3) both produced colored powders, which after annealing afforded nanocrystalline InP particles with respective purities of 91.53% and 93.08% and average domain size of approximately 4 nm for both samples. The 1:1 mole ratio reaction of InI3 with P(SiMe(3))(3) afforded the 1:1 adduct I3In . P(SiMe(3))(3) (1). Compound 1 crystallizes in the monoclinic system, space group P2(1)/c, with a = 16.074(7), b = 9.730(3), c = 16.454(6) Angstrom, V = 2362.1(15) Angstrom(3), D-calc = 2.098 g cm(-3) for Z = 4; the In-P bond length is 2.537(3) Angstrom. Decomposition of 1 affords nanocrystalline InP of 84.06% purity with an approximate average domain size of 2.5 nm.