Abstract Mechanically alloyed (MA) AlTi and AlOTi complexes have been studied by X-ray absorption fine structure (XAFS) at the Ti K-edge. In the MA mixture of Al and Ti, the single pre-edge peak due to the electron transition 1s → 3d disappears, and the intensity of the first nearest neighbor peak in the EXAFS structure function ¦ F(r)¦ decreases. In the MA mixture of Al and TiO 2 hydrogel, the number of pre-edge peaks apparently decreases from three to one. At the same time, the intensity of the ¦ F(r)¦ peak due to the first nearest neighbor increases, and its position approaches that of Al 2TiO 3. Similar phenomena are observed in the MA mixture of Al 2O 3 and TiO 2 hydrogels. These results suggest that mechanical stressing causes characteristic electronic interaction and the reconstruction of short-range order through intimate mixing at an atomic level. This accords with our previous NMR studies.