Iron niobate (FeNbO
4) nanospheres of an orthorhombic structure were synthesized using a hydrothermal (HT) process at 250°C, and were characterized using X-ray diffraction, field-emission scanning electron microscopy, high-resolution transmission electron microscopy, and Brunauer–Emmett–Teller (BET) measurements. The FeNbO
4 nanospheres obtained through the HT reaction revealed a uniform size with an average diameter of 5–10 nm, and a larger specific surface area (82.72 m
2 g
−1) than that of bulk FeNbO
4 powder (2.51 m
2 g
−1) prepared by a solid-state reaction. In addition, the electrochemical properties of the FeNbO
4 powders versus Li were evaluated using cyclic voltammetry and galvanostatic charge/discharge cycling. Importantly, the FeNbO
4 nanospheres delivered a reversible capacity of over 200 mAh g
−1 after 20 cycles, and provided an enhanced rate capability compared to the bulk material.
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