Pore-free bulk samples were produced by HERF axisymmetrical powder compaction for different application purposes in case of the immiscible At and Pb metal pair. The Al-Pb nanocomposites were made by mechanical milling of atomised At and Pb powders in air. The nano Pb and PbO particles were shown by SEM, XRD and TEM (BF, DF, SAED) using the ProcessDiffraction method. (c) 2005 Elsevier B.V. All rights reserved.