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We present a unique composite assembly of rhombohedral Li3V2(PO4)3 and carbon nanofiber, which simultaneously facilitates Li-ion transport as well as electron transfer. For the synthesis of this composite, the inorganic precursors were confined in electron-spun nanofibers, and then, through controlled annealing, Na3V2(PO4)3 particulates were grown with controllable crystallite size and partially embedded into carbon nanofibers with precisely controlled diameter. The rhombohedral Li3V2(PO4)3 could be successfully obtained by ion exchange from Na to Li in the

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