Precursors to alloys such as Bi2SeTe2, Bi0.5Sb1.5Te3, and Bi1.8Sb0.2Se0.15Te2.85 are synthesized by aqueous coprecipitation and metal-organo complex methods. The alloys are produced in fine-powder, polycrystalline form by hydrogen reduction of the precursors. Identification of the alloys is supported by total elemental analysis and X-ray diffraction data. The approach is simpler than conventional melt processing and gives product yields in the 88-92% range.