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LiFe 1−y Mn y PO 4 /C nanofi ber composites are applied as cathode materials in Li-ion batteries and their electrochemical properties are explored. Nanofi ber meshes are synthesized via electrospinning of commercially available precursors (LiOH · H 2 O, FeSO 4 · 7H 2 O, MnSO 4 · H 2 O, H 3 PO 4 , and polyvinylpyrrolidone). Nanofi bers calcined at 850 ° C under Ar/H 2 (95/5 vol%) atmosphere are directly used as self-supporting electrodes in Swagelok half cells without the need for any conductive additive or polymer binder. The morphology, phase, and chemical composition of as-prepared and heat-treated samples are analyzed by means of X-ray powder diffraction, thermogravimetric analysis, and electron and scanning microscopy techniques. Brunauer-Emmett-Teller gas adsorption-desorption measurements show a high specifi c surface area (111m 2 g − 1 ) for LiFe 0.5 Mn 0.5 PO 4 . The infl uence of different Fe/Mn ratios on the morphology, electrical, and electrochemical performances are analyzed. 554 www.MaterialsViews.com www.advenergymat.de