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              <p>A novel two-step strategy to prepare amorphous oxyfluorides, containing both divalent and trivalent 3d-metals, as cathode materials for lithium batteries is presented. The first step involves the preparation of hydrated fluorides M2+M3+2F8(H2O)2 (M2+ = Mn, Fe, Co, Ni, Cu; M3+ = V, Fe) by microwave-assisted solvothermal synthesis. Besides the MnFe2F8(H2O)2 and CuFe2F8(H2O)2 phases, three new compounds, Fe1.3V1.7F8(H2O)2, CoFe2 F8(H2O)2, and Ni- Fe2F8(H2O)2, which are isostructural with Fe3F8(H2O)2, have been unraveled. The second step consists in the decomposition of M2+M3+2F8(H2O)2 into amorphous oxyfluorides M2+M3+2F8−2xOx via suitable thermal treatments.. The amorphous materials show a greater electrochemical activity toward Li than their parent phases, among them being CuFe2F6O, which displays the best performance as a cathode material with a first discharge capacity of 310 mAh·g−1. We show that such a large capacity results from cumulative insertion and displacement reactions.</p>
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