A mechanical alloying technique has been applied for Nd-Fe-B alloy synthesis from the mixture of neodymium, iron and Fe-B powders. The direct formation of Nd2Fe14B phase (phi phase) was not observed, but an Nd-Fe multilayer structure was formed during the milling process. Annealing of milled powders at 1023 K for 1 h resulted in magnet formation. The dependence of the magnetic properties on milling time was observed. For the applied milling device and parameters, the optimum milling time proved to be 4 h and the coercive force reached a value of about 1000 kA m(-1).