Solid–solid and gas–solid interactions induced during high-energy milling to produce PbTe nanopowders

Transformations from precursors to nanoparticles by high-energy milling are promoted by two major driving forces, namely physical and/or chemical. While the former has been difficult to trace since stress, strain and recovery may occur almost simultaneously during milling, the latter has been sequentially followed as an evolution from precursors to intermediate phases and thereof to high purity nanocrystals. The specific objective of this work is to discern how solid–solid and partially solid–gas reactions manifest themselves correspondingly as a short-range diffusion through an interface or how vapor species, as a subliming phenomenon, grows as a different phase on an active local surface. These series of changes were traced by sub-cooling the as-milled powders extracted during a milling cycle. Through this experimental technique, samples were electron microscopically analyzed and where it was required, selected area electron diffraction images were obtained. High-resolution transmission electron microscopy results, unambiguously, confirm that nanocrystals in the last stage show a cubic morphology which average size distributions are around 17 nm.