Nano-size particles and composites as anode materials have been explored in recent years in order to reduce the cost, improve the capacity as well as cycle-life of the Lithium ion batteries (LIBs). In view of same, the nanofibers of spinel-NiCo2O4 are prepared by easy, viable and cost effective electrospinning technique. The as spunned nanofibers composed of polymer solution and metal precursors are sintered at various temperature, and 5000C. 2h is found to be the appropriate to get best crystalline nanofibers of spinel-NiCo2O4. The structural, morphological and thermal characterizations are carried out by XRD, FESEM, TGA, respectively. The Li-storage and cycling properties of optimized nano-fibers of NiCo2O4 are examined by means of galvanostatic cycling and cyclic voltammetry. The spinel-NiCo2O4 delivers the first discharge and charge capacities of 1220(±10) mAhg−1 and 910(±10) mAhg−1 that corresponds the consumption of 11.0 and 8.2 mole of Li, respectively. The cyclic voltammetry studies reveal the average charge and discharge potentials of ∼2.2 and ∼0.9 V, respectively. Based on galvanostatic cycling, cyclic voltammetry and ex-situ studies like XRD, TEM and SAED, a plausible reaction mechanism is proposed.

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