Abstract: There is disclosed a process for preparing a thallium-containing superconductive composition. In the first step of the process, a mixture of an inorganic salt (such as potassium chloride) and a powder compositon is provided; the powder composition contains at least three separate compounds which, in combination, correspond to the stoichiometry of the super-conductor to be produced. This mixture is then charged to a closed container, raised to a temperature of from 800-959 degrees Centigrade, and heated for from about 1 to about 12 hours; thereafter, it is cooled to a temperature of 600 degrees Centigrade at a rate of at least 300 degrees Celsius per hour.