Nd 25 Fe 40 Co 20 Al 10 B 5 was prepared by high-energy milling and melt-spinning techniques. The as-milled and as-quenched samples were subsequently annealed in a temperature range from 400to1100°C for 20min. For the annealed samples, x-ray diffraction combined with high-resolution transmission microscopy show the presence of ferromagnetic Nd2(Fe,Co,Al)14B crystallites coexisting with antiferromagnetic Nd6(Fe,Co,Al)14 ones, among an amorphous matrix. After annealing, coercivities of about 22 and 25kOe can be reached with the high-energy milled and melt-spun samples, respectively, while the Curie temperature of both samples reaches 660K.