Iron antimony oxide (FeSbO4) with specific surface area (SSA) over 50 m(2)/g was synthesized mechanochemically by milling a mixture of iron oxy-hydroxide (FeOOH) and antimony pentoxide (Sb2O5) using a planetary ball mill at room temperature. The mechanochemical reaction proceeds with an increase in milling time and has been completed by 120 min. The prepared product powders are in the state of agglomerates consisted of fine particles of several dozen nanometers. This method has been extended to synthesis of FeSbO4-based materials with different Fe/Sb atomic ratios (1 <= Fe/Sb <= 4). The SSA value of these prepared samples is in the range of 50 to 65 m(2)/g. (c) 2007 Elsevier B.V. All rights reserved.