Freestanding, flexible Fe2O3-SnOx-CNF mats were fabricated by electrospinning. The optimized concentrations of Fe2O3 and SnOx presented to get higher capacity. A reversible capacity of CNF with 3:1 Fe:Sn ratio is 756 mAh·g−1 after 55 cycles. The 3:1 Fe:Sn ratio shows high capacity of 540 mAh·g−1 at 1A·g−1 current rate.