Abstract In the current study, pure elemental powders of Fe and S were mixed to give the desired compositions of Fe67S33, Fe50S50 and Fe33S67. A SPEX 8000D high-energy ball mill was used to synthesize iron sulfide powders under an Ar-filled atmosphere. The as-milled powders were examined by conventional X-ray diffraction (XRD) and synchrotron X-ray absorption spectroscopy (XAS). The experimental results showed that mechanochemical reactions occurred during the ball mil領 process for all the compositions investigated. The Fe1−xS phase was observed at the end of mil領. The formation time of the Fe1−xS phase increased with increasing sulfur content. Extended X-ray absorption fine structure (EXAFS) results revealed that the nearest neior bond lengths of the radial distribution function for iron decreased when iron sulfides formed. X-ray absorption near-edge structure (XANES) of sulfar K-edges distinguished better the structural evolution of these iron sulfides. © 2003 Elsevier B.V. All rights reserved. SPEX8000D 高能量球磨機