A precipitation process has been developed to prepare precursor powders, which can be calcined and sintered to form high‐Tc superconductors such as YBa2Cu3Oy. Precursor powders are prepared using a mixed‐precipitants system in which a solution contains precipitating anions such as hydroxide, oxinate and oxalate ions. A theoretical study on the conditions of mixed‐precipitants coprecipitation is performed. The solution pH of complete precipitation of the title system is extended and is maintained between 4.46 and 12.0. A series of experiments were conducted to confirm the as‐derived optimal condition. Finally, characterization of the properties of the YBa2Cu3Oy obtained after high temperature treatment is reported.