Electron microscopy nanoscale characterization of ball-milled Cu–Ag powders. Part I: Solid solution synthesized by cryo-milling

Abstract

We present a study of nanostructured Cu–Ag material obtained by low temperature ball milling. The microstructural characterization is carried out using a wide variety of transmission electron microscopy (TEM) techniques from conventional dark-field imaging, selected area diffraction and energy dispersive X-ray spectrometry (EDS) to more modern techniques of scanning TEM high-angle dark-field imaging (HAADF), nanodiffraction and high resolution imaging (HREM). A novel method of HREM image analysis is also presented which consists of calculating geometric phase images by Fourier filtering. Real-space maps of lattice spacings and lattice rotations are thus obtained. The analysis addresses the following essential points of nanostructural characterization: dislocation densities, grain sizes and morphologies, grain boundaries and local lattice rotations, local textures, local variations in lattice parameters. A new description of the microstructure emerges from the observations, quite different to that expected. Analytical modeling suggests that large lattice rotations can be expected in nanomaterials produced by intense deformation.