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   <subfield code="a">Metastable antimony(V) oxide compounds are prepared via mechanochemical reactions in mixtures of CaO and Sb2O3, followed by mild oxidizing heat treatment and calcium leaching in a hydrochloric acid solution, and are characterized by x-ray diffraction and thermal analysis. The synthesized compounds have the pyrochlore structure or a monoclinic pyrochlore-like structure (Ca16Sb 3+ 8 Sb 5+ 8 O48). Doping with fluorine slows down subsequent oxidation, while doping with lanthanum impedes calcium leaching. The composition and morphology of the powders (nanopores and core-shell microstructure of the grains) determine their properties: water release in a broad temperature range, proton conductivity, and low absorption capacity for Na+ ions. In hydrogen atmosphere, the reduction of antimony decreases their conductivity.</subfield>
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