In this paper, we report on the preparation of synthetic FeS2 and CoS2 using a relatively inexpensive aqueous process. This avoids the material and handling difficulties associated with a high-temperature approach. An aqueous approach also allows ready scale-up to a pilot-plant size facility. The FeS2 and CoS2 were characterized with respect to their physical and chemical properties. The synthetic disulfides were incorporated into catholyte mixes for testing in single cells and batteries over a range of temperatures. The results of these tests are presented and compared to the performance of natural FeS2 (pyrite) and a commercial source of CoS2.