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Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3-δ perovskite-type compounds are well-known mixed ionic-electronic conductors for oxygen electrocatalytic applications, although their performance is strictly dependent on the selected preparation methodology and processing parameters. The reducers-to-oxidizers ratio (Φ) is a very important parameter in the solution combustion synthesis of mixed ionic-electronic conductors. Selection of Φ is not trivial and it strongly depends on the type of fuel used, the chemical composition and the specific application of the material. This work clarifies the role of Φ in the solution combustion synthesis of Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3-δ for application as oxygen electrocatalysts. Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3-δ powders were synthesized by solution combustion synthesis using sucrose-polyethylene glycol fuel mixtures with reducers-to-oxidizers ratio values between 1 (stoichiometric) and 3 (over-stoichiometric). Chemical-physical properties were studied by X-ray diffraction, scanning electron microscopy, N₂ adsorption at −196 °C, H₂-temperature programmed reduction and thermogravimetric analysis. The results evidenced the direct role of Φ on the intensity and redox environment of the combustion process, and its indirect influence on the Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3-δ electrode materials properties. Taking into account the general picture, the highly over-stoichiometric Φ was selected as the optimal one and the electrochemical activity of the corresponding powder was tested by electrochemical impedance spectroscopy on electrolyte-supported half-cells employing a Ce_0.8Sm_0.2O_2-x electrolyte. Full article

The methodologies and experimental conditions used for the synthesis of cathode materials for electrochemical devices strongly influence their electrocatalytic performance. In particular, solution combustion synthesis is a convenient and versatile methodology allowing a fine-tuning of the properties of the material. In this work, we used for the first time a sucrose assisted-solution combustion synthesis for the preparation of Cerium and Cobalt-doped SrFeO_3–δ electrocatalysts and we investigated the effect of polyethylene glycol (PEG) addition as a secondary fuel on their structural, microstructural, redox and electrochemical properties. The perovskite-type powders were characterized by X-ray diffraction coupled with Rietveld refinement, scanning, and high-resolution transmission electron microscopies, thermogravimetric analysis, nitrogen adsorption measurements, and temperature-programmed reduction. Electrical conductivity and overpotential measurements were performed after the deposition of the powders onto a Gd-doped ceria electrolyte pellet. Stable high-valence B-site cations were detected in the powders prepared from sucrose-PEG fuel mixtures, although a substantial improvement of the conductivity and a decrease of the overpotential values were obtained only with high molecular weight PEG. The superior electrochemical performance obtained using PEG with high molecular weight has been ascribed to a faster interaction of the powder with the oxygen gas phase favored by the nanometer-sized crystalline domains. Full article