The process of macro- and microstructural transformations of zinc-oxide powders, which were tribophysically activated by grinding in a vibro-mill was investigated using methods of transmission electron microscopy, infrared spectroscopy and X-ray. It is shown that tribophysical activation contributes to a gradual modification of the fine defect structure of zinc-oxide powders. In the starting stage agglomerates and bigger, longer particles are destroyed first of all. As a result of the formation of both volume and surface defects and changes of the character of interparticles interactions the plate-like polycrystal particles are created. They actually present sets of coherent scattering region.