Aerosol Spray Pyrolysis (ASP) was employed for the synthesis of oxygen-deficient doped ferrite systems to be used as redox materials for the production of solar Hydrogen from water via a two-step thermochemical water-splitting cycle. Redox materials of the iron spinel family doped with other bivalent metals were synthesized in the temperature range 350-1070 °C, characterized and evaluated with respect to their watersplitting activity. The very short synthesis times and high cooling rates were capable of producing particles with high and “tunable” defects (oxygen vacancies) concentration that can be more active water-splitters. Organic additives in the precursor solutions were found to enhance the materials water-splitting activity. Material performance (water splitting activity, hydrogen yield, regeneration capability) was found to depend on the dopants' kind and stoichiometry. ASP synthesized materials have demonstrated higher water conversion and hydrogen yield from materials of the same composition synthesized through solid-state routes. The ASP synthesis process was scaled-up successfully maintaining the favourable characteristics of the synthesized materials.
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