Lattice distortion in nanocrystalline Fe powder studied by positron annihilation and X-ray diffraction

Abstract

X-ray diffraction and positron annihilation measurements were performed on the ball-milled nanocrystalline Fe powder over a wide range of crystallite sizes (9–90 nm). With increasing milling time, the crystallite size reduction was accompanied by a monotonic increase of the lattice parameter of Fe (i.e. lattice expansion). The positron lifetime increased significantly due to enhanced positron annihilation from the defects (excess vacancies, vacancyclusters, etc.) generated at the Fe grain boundaries and intercrystalline regions with progressive milling up to 24 h (crystallite size ∼ 12 nm). The observed lattice expansion has been successfully simulated using a theoretical model taking account of the excess free volume associated with the excess vacancies/vacancy-clusters at the grain boundaries in nanocrystalline Fe. Prolonged ball milling up to 36 h (crystallite size < 10 nm) led to an anomalous decrease of all positron lifetime parameters. The X-ray diffraction line profiles of ball-milled Fe powder exhibited anisotropic broadening due to the high density of dislocations in Fe. Milling duration ≥ 24 h further led to asymmetric broadening of Fe diffraction peaks indicating heterogeneous dislocation structure in the severely plastically deformed ball-milled Fe. Further analysis of asymmetrically broadened peak reflections revealed deformation induced tetragonal distortion of body centered cubic Fe lattice in the 36 h ball-milled Fe powder.