P. Boudjouk et al., BIS(TRIPHENYLTIN) CHALCOGENIDES AS CONVENIENT PRECURSORS TO PHASE-PURE BINARY SEMICONDUCTORS, Chemistry of materials, 6(11), 1994, pp. 2108-2112
Bis(triphenyltin) chalcogenides, (Ph3Sn)2X (X = S, Se, and Te), were s
ynthesized in good yield from Ph3SnCl and anhydrous Na2X made from ele
mental Na and X with a catalytic amount of naphthalene in THF. When he
ated to relatively modest temperatures (above 300-degrees-C) under an
inert atmosphere, it is observed that these compounds undergo a series
of phenyl migrations in the condensed (liquid) state. This pyrolysis
results in the loss of tetraphenyltin and diphenylchalcogen as ''volat
ile'' byproducts while leaving behind an inorganic powder. These powde
rs are characterized by X-ray diffraction and found to be phase pure a
nd highly crystalline SnS, SnSe, or SnTe. Combustion analysis detects
less than 1% carbon contamination after rinsing with common solvents.
Scanning electron micrographs show the powders to be polycrystalline a
gglomerates having platy (SnS and SnSe) or cubooctahedral (SnTe) habit
s.