Nanocrystalline materials, which are defined as materials with grain sizes less than 100 nm have received much attention as advanced materials with improved physical and mechanical properties [1] . Mechanical alloying (MA) is one of the solid state reaction techniques by which novel materials may be synthesized from elemental or prealloyed powders. Mechanical alloying involves the synthesis of materials by high-energy ball milling. It was first developed by John Benjamin to produce oxide dispersion strengthened materials [2] . Furthermore, mechanical alloying has been reported to be capable of producing non-equilibrium structures including amorphous alloys, nanocrystalline materials and extended solid solutions [3][4][5] . It is also used to obtain alloys subjected to ulterior annealing and consolidation [6 and 7] . Over the past several decades, amorphous and more recently nanocrystalline Fe-based materials have been investigated for applications such as telecommunications, power electronics, micro devices, and so on [8 and 9] .Although it is known that Fe-based alloys prepared by rapid solidification techniques, in ribbon form, can exhibit superior soft magnetic properties [10] , they do not attain a more significant level of applicability because its shape limits their technological use. Mechanical alloying of ribbons is recently applied as an alternative route to obtain powdered materials [11 and 12] . If the original material is amorphous, controlled annealing D De ev ve el lo op pm me en nt t o of f F Fe e--b ba as se ed d n na an no oc cr ry ys st ta al ll li in ne e m ma at te er ri ia al ls s b by y m me ec ch ha an ni ic ca al l a al ll lo oy yi in ng g ( (· ·) ) J.J. Suñol*, A. González*, L. Escoda* and M.T. Mora** A Ab bs st tr ra ac ct t Two alloys, Fe 80 Nb 10 B 10 and Fe 70 Ni 14 Zr 6 B 10 , were produced by mechanical alloying. The formation of the nanocrystallites (about 7-8 nm at 80h MA) was detected by X-ray diffraction. After milling for 80 h, differential scanning calorimetry scans show low-temperature recovery processes and several crystallization processes related with crystal growth and reordering of crystalline phases. The apparent activation energy values are 315 ± 40 kJ mol -1 for alloy A, and 295 ± 20 kJ mol -1 and 320 ± 25 kJ mol -1 for alloy B. Furthermore, a melt-spun Fe-based ribbon was mechanically alloyed to obtain a powdered-like alloy. The increase of the rotation speed and the ball-to-powder weight ratio reduces the necessary time to obtain the powdered form. , han sido producidas por aleado mecánico. Mediante difracción de rayos X se ha detectado la formación de nanocristales (7-8 nm a las 80 h de aleado). Tras molturar 80 h, las curvas calorimétricas muestran procesos exotérmicos asociados a la relajación estructural y al crecimiento cristalino y reordenación de la fase cristalina. Los valores de la energía aparente de activación de las cristalizaciones son 315 ± 40 kJ mol -1 para la aleación A, y 295 ± 20 kJ mol -1 y 320 ± 25 kJ mol -1 para la aleación B. Por otra parte...