One of the leading production method to create nanostructured materials for thermal spray applications is mechanical alloying. The mechanical milling process is a high-energy ball milling technique that produces materials at nanometric level. This paper reviews the main techniques to obtain nanomaterials and describes the synthesis of the nanocrystalline NiCrAlY powder by mechanical cryomilling. The microstructure and morphology of the nanostructured NiCrAlY powders were characterized by XRD, SEM and TEM. (C) 2004 Elsevier B.V. All rights reserved.