Multi-electron reaction anodes have been exciting battery materials due to their exceptionally high energy densities. Herein, nanostructured iron borides (nanoFeB) have been synthesized via dip-coating chemical reduction in conjunction with a heat treatment procedure and were directly used as anodes in a metal/metalloid-air battery. The crystal structure, particle size, BET surface area, and electrochemical properties of iron boride samples treated at four different temperature conditions (200 degrees C, 300 degrees C, 400 degrees C, and 500 degrees C) were investigated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N-2 adsorption-desorption isotherms, potentiodynamic polarization, and electrochemical impedance spectroscopy (EIS). The nanoFeB heat-treated at 300 degrees C (nanoFeB(300)) exhibits the highest surface area among reported values in literature and demonstrates excellent anode discharge performance in a metal/metalloid-air battery. (C) 2016 Elsevier B.V. All rights reserved.