Combustion synthesis, structural and magnetic characterization of Ce1−xPrxO2 system

Abstract

The current work describes the synthesis of Ce1−xPrxO2 (x = 0.0, 0.2, 0.4, 0.6, 0.8) and Pr6O11 systems by the combustion method, using citric acid as chelating agent. The obtained solids after combustion and calcination processes were characterized by thermal analysis (TGA-DTA) and infrared spectroscopy (FT-IR) to evaluate the chemical process during the combustion reaction. The surface area analysis using isotherms of nitrogen adsorption, reveal that all samples exhibit values between 70 and 135 m2 g−1, with a pore volume that allows its classification as mesoporous materials. The structural analysis by X-ray diffraction (XRD) and Rietveld refinement, revealed the obtention of a pure cubic structure Fm3m (225) along all cerium oxide modifications with nanocrystalline domain sizes, except for the praseodymium oxide that shows two crystalline phases in a monoclinic crystalline phase P12 1 /c 1 (14) in the case of Pr6O11 and a cubic phase Fm3m (225) for PrO2 oxide. The oxygen storage capacity measurements performed in all samples, demonstrate that exchange of Ce ions by Pr increases the storage capacity of samples over the reference values in accordance with the synthesis method. The characterization by high-resolution transmission electron microscopy, confirmed that the solids are composed by nanometric aggregates with d spacing between 0.29 and 0.31 nm along main diffraction signals, in accordance with the experimental XRD results. Finally, the magnetic characterization in a ZFC configuration and a M-H mode, shows a strong paramagnetic behavior in all systems except in CeO2 oxide, which exhibited a prevalent diamagnetic behavior.