One-step hydrothermal method was developed to prepare hybrid gamma-Fe2O3/carbon hollow spheres with a predominant orientation (111) plane of gamma-Fe2O3 and rich oxygen-containing functional groups on carbon. The resulting functional hybrid exhibited extremely high adsorption capacities for toxic Pb(II) and Cr(VI) ions in solutions with easy magnetic separation. The ease of synthesis and low cost, coupled with the efficient and rapid removal of toxic heavy metal ions, make hybrid gamma-Fe2O3/carbon hollow spheres an attractive adsorbent for the purification of waste and contaminated water. (C) 2014 Elsevier Inc. All rights reserved.