Abstract: Stoichiometric titanium disulfide having a high degree of crystalline perfection and particularly suited for use as an active cathode material is prepared by heating particulate metallic titanium to a reaction temperature between about 475.degree. and 600.degree. C., contacting the heated titanium with an atmosphere having a sulfur partial pressure substantially equal to the equilibrium sulfur partial pressure at the reaction temperature to form titanium disulfide, and maintaining the reactants at the reaction temperature sufficiently to insure complete reaction. The reaction is advantageously conducted in an evacuated tube which is differentially heated to establish a hot zone where the reaction occurs and a cooler zone which controls the sulfur partial pressure within the tube so that the rate of reaction can in turn be controlled to minimize overheating, and also prevents the formation of titanium trisulfide.