An EXAFS (extended x-ray-absorption fine structure) study of nanocrystalline iron prepared by high-energy ball milling is presented. Accurate data analysis has been performed using a recently developed ab initio multiple-scattering method (GNXAS). The crystalline iron EXAFS spectrum, taken as reference, has been analyzed taking proper account of the important multiple-scattering signal. Results of the data analysis are shown to be in good agreement with known structural values. The dramatic decrease of the first-neighbor coordination number found in nanocrystalline iron, as a function of the milling time, is shown to be related to the presence of a large defect density. The corresponding decrease of the coordination numbers of the second and further neighbors, as well as the significant decrease of the multiplicities of the three-atom configurations, confirms this interpretation. A simple model which takes into account the presence of atomic defects is shown to lead to marked reduction of coordination numbers and three-atom multiplicities in agreement with the experimental data. Selected models without lattice defects are shown to be unable to give a quantitative explanation of the intensity reduction of the EXAFS signal found in milled nanocrystalline iron. An in situ annealing of the sample (up to about 1100 °C) milled for the longer time (32 h) is shown to reduce considerably the density of the defects, as expected, although no complete recovering of the crystalline order is found. The transition from α iron to γ iron has been directly observed for such nanocrystalline material.

• Received 12 April 1994

DOI:https://doi.org/10.1103/PhysRevB.50.12386