Controlled redox reactions during spray pyrolysis of the YBa2Cu3O(7- x) ("123") are described and subsequent use of the as-prepared powders in thick films is illustrated. The highly exothermic reaction between the metal nitrate precursors and organic fuels is utilized in the continuous production of "123" precursor powders. As-prepared powders may be tape-cast and reactively sintered or subsequently calcined in air to form single-phase powders.