In this work, bare and Ta-substituted Nb2O5 nanofibers are prepared by electrospinning followed by sintering at temperatures in the 800-1100 degrees C range for 1 h in air. Obtained bare and Ta-substituted Nb2O5 polymorphs are characterized by X-ray diffraction, scanning electron microscopy, density measurement, and Brunauer. Emmett and Teller surface area. Electrochemical properties are evaluated by cyclic voltammetry and galvanostatic techniques. Cycling performance of Nb2O5 structures prepared at temperature 800 degrees C, 900 degrees C, and 1100 degrees C shows following discharge capacity at the end-of 10th cycle: 123, 140, and 164 (+/- 3) mAh g(-1), respectively, in the voltage range 1.2-3.0V and at current rate of 150 mA g(-1) (1.5 C rate). Heat treated composite electrode based on M-Nb2O5 (1100 degrees C) in argon atmosphere at 220 degrees C, shows an improved discharge capacity of 192 (+/- 3) mAh g(-1) at the end of 10th cycle. The discharge capacity of Ta-substituted Nb2O5 prepared at 900 degrees C and 1100 degrees C showed a reversible capacity of 150, 202 (+/- 3) mAh g(-1). respectively, in the voltage range 1.2-3.0V and at current rate of 150 mA g(-1). Anodic electrochemical properties of M-Nb2O5 deliver a reversible capacity of 382 (+/- 5) mAh g(-1) at the end of 25th cycle and Ta-substituted Nb2O5 prepared at 900 degrees C, 1000 degrees C and 1100 degrees C shows a reversible capacity of 205, 130 and 200 (+/- 3) mAh g(-1) (at 25th cycle) in the range, 0.005-2.6V. at current rate of 100 mA g(-1). (C) 2010 Elsevier Ltd. All rights reserved.