Phase transformation during Sr2CrMoO6–δ synthesis

Abstract

The sequence of phase transformations in the process of crystallization of the Sr 2 CrMoO 6 by the solid-phase technique from a stoichiometric mixture of simple oxides SrCO 3 + 0.5Cr 2 O 3 + MoO, has been investigated. It was determined that the synthesis of the strontium chrome-molybdate proceeds through a series of sequential-parallel stages. By means of the differential thermal analysis and thermogravimetric analysis data, it has been established that five clearly expressed endothermal effects were observed in the temperature range 300—1300 K. It was found that during the studies of the phase transformations sequence in the process of the double perovskite synthesis, SrCrO 3 , SrMoO 4 and Sr 2 CrO 4 are the main concomitant compounds. Herewith, it has been observed that with the annealing temperature increase from 300 to 1270 K, the complex compounds SrCrO 4 , SrCrO 3 (350—550 K) and SrMoO 4 , Sr 2 CrO 4 (600—750 K) are emerging initially and practically simultaneously. It has been revealed with a subsequent temperature increase that in the temperature range 940—1100 K, the SrMoO 4 , Sr 2 CrO 4 and SrCrO3 phase concentration dramatically drops with the emerging and growth of the Sr 2 CrMoO 6-δ double perovskite. With that in the range up to 1120—1190 K, the main XRD reflexes intensity for the SrCrO 3 and SrMoO 4 lowers substantially, and their content in the samples at 1170 К is no more than 7,9 %. During a consideration of the derivative of the SrCrO 3 , SrMoO 4 and Sr 2 CrO 4 phase transformation degree (|(dα/dt)|mах), at which their crystallization rates are maximal, it has been determined that |(dα/dt)| mах for the Sr2CrO4 corresponds to the maximal temperature 1045 K, which indicates the presence of considerable kinetic difficulties at the formation of the Sr 2 CrO 4 phase. Thereafter this phase does not disappear and at its appearance the slowing down of the double perovskite growth takes place. On the base of investigations of the phase transformations dynamics for the obtaining of the single-phase Sr 2 CrMoO 6-δ compound with the superstructural ordering of the Cr/Mo cations and improved magnetic characteristics, the SrCrO 3 and SrMoO 4 precursors were used with combined heating modes.