Abstract
The process of nanocrystalline structure formation during mechanical milling was studied in Al and Fe powders. A detailed microstructural study of powder samples was carried out by X-ray diffraction experiments as a function of milling time. As a result, nanosized powders have been synthesized with microstructures showing a significant decrease of the coherent diffraction domains and the creation of a large number of linear defects, which induce microstrains. SEM results show that welding of very small particles to the surfaces of larger particles occurred and that the powder particles tended to form a matrix of randomly welded thin layers of highly deformed particles. Calorimetric measurements, as a function of milling time, indicated the decrease of the melting point of Al powder and at early stages it can be seen that initially endothermic peak was divided to two endothermic melting peaks. This is probably due to the oxide layer around the Al grains. In the case of Fe powder, the DSC measurements show a broad exothermal peak occurring over quite a large temperature interval, corresponding to the strain release and grain growth. (c) 2007 Elsevier Inc. All rights reserved.