Carbon Nano Fibers (CNFs) coated with LiFePO4 particles have been prepared by a non-aqueous sol–gel technique. The functionalization of the CNFs by HNO3 acid treatment has been confirmed by Raman and XPS analyses. The samples pure LiFePO4 and LiFePO4–CNF have been characterized by XRD, SEM, RAMAN, XPS and electrochemical analysis. The LiFePO4–CNF sample shows better electrochemical performance compared to as-prepared LiFePO4. LiFePO4–CNF (10wt.%) delivers a higher specific capacity (∼140mAhg−1) than LiFePO4 with carbon black (25wt.%) added after synthesis (∼120mAhg−1) at 0.1C.