Nanocomposite powders were produced by high energy ball milling of the Al50-Fe25-Ti25 (at.%) powder mixture added with ethanol (C 2 H 5 OH) and ammonium carbonate ((NH 4 ) 2 CO 3 ). The phase transformations occurring in the material during the process were monitored by X-ray diffractometry and the structures of the milled samples were examined using transmission electron microscopy. The nanocrystalline composite powder consisting of complex (Ti,Al)C carbide distributed in the Fe(Al) matrix was obtained as the final product of the milling with participation of ethanol whereas the process performed with an addition of ammonium carbonate led to the formation of (Ti,Al)N-Fe(Al) nanocomposite.