The sol-gel-type condensation of tin(1V) ethoxide [Sn(OEt),], (where OEt is ethoxide) under basic conditions produced spherical, submicrometer-sized tin(1V) oxide (cassiterite) particles. Transmission electron microscopy and powder X-ray diffraction data indicated that the grain size was approximately 20 to 30 A (2 to 3 nm). The mixed-metal alkoxide compound [ZnSn(OEt)s] was hydrolyzed under analogous conditions to give either spherical or octahedral submicrometer-sized crystalline particles of ZnSn(0H)r depending on the solvents used. These data demonstrated that the stoichiometry of the mixed-metal alkoxide precursor was retained during Condensation. Thermal treatment of ZnSn(OH)6 resulted in crystallization of ZnSn03 at approximately 676°C. At neutral pH, hydrolysis of [ZnSn(OEt)6] resulted in formation of a high surface area (261 m2/g) amorphous powder. [
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A series of transition metal substituted germacyclopent-3-ene compounds containing transition metal-germanium bonds have been prepared with supporting ligands which are designed to be easily removed either thermally or photochemically. In solution, model thermal decomposition experiments show that either the geramanium or the transition metal substituents may be removed, depending on the nature of the metal. Preliminary hot-wall CVD experiments using manganese and cobalt derivatives result in films with small grain size.
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