This paper reports a new way to synthesize the BaBi1/2Sb1/2O3 perovskite-type compound with high purity. The method is based on the initial preparation of barium oxalate hydrate (Ba(COO)(2)(.)0.5H(2)O) and antimony oxalate hydroxide (Sb(COO)(2)(OH)) and the subsequent calcination of an equimolar physical mixture of the oxalates and Bi2O3 oxide. The thermal decomposition of both the oxalates and the formation of single-phase BaBi1/2Sb1/2O3 by calcination was investigated by X-ray powder diffraction (XRPD) and differential thermal analysis (DTA). The formation temperature of BaBi1/2Sb1/2O3 was estimated as 950 degrees C. (c) 2005 Elsevier B.V. All rights reserved.