(Co,Fe)Pt alloy nanoparticles of Al-type structure were obtained by reduction of metallic salts by hydrazine in aqueous medium. Sb and Cu were used as additives for the (Co,Pt) and (Fe,Pt) systems, respectively. Sols of CoPt particles capped with oleylamine were obtained in one step by achieving the synthesis in an H2O/hexane two-phase medium. Conversion to an L1(0) phase was investigated in powders. (c) 2004 Elsevier B.V. All rights reserved.