Al-La-Ni-Fe alloys of three different compositions (Al82La10Ni4Fe4, Al85La9Ni3Fe3 and Al88La6Ni3Fe3) were prepared high-energy milling in a planetary ball-mill (AGO-2). Complete amorphization was observed for the Al82La10Ni4Fe4 alloy after milling for 350 h at a rotational speed of 300 rpm. In contrast, the Al85La9Ni3Fe3 and Al88La6Ni3Fe3 powders contained the FCC Al phase even for prolonged milling. The amorphization tendency was found to increase in the order of Al88La6Ni3Fe3 < Al85La9Ni3Fe3 < Al82La10Ni4Fe4, which may well be ascribed to the increasing atomic size mismatch of the constituent elements on La addition. DSC analyses of amorphous samples revealed two-stage crystallization processes for all three alloys, however, with strong variations in the thermal stability upon compositional changes. As observed by SEM, amorphous powders consisted of particles with nearly spherical shape and diameters ranging from 5 to 20 µm.