The crystallization kinetics of amorphous (Nd_(3.6)Pr_(5.4)Fe_(83)Co_3B_5) and the preparation of α-Fe/Nd_2Fe_(14)B nanocomposite magnets by controlled melt-solidification of (Nd_(3.6)Pr_(5.4)Fe_(83)Co_3B_5) was investigated by employing DTA, XRD, and TEM. The results show that a metastable intermediate phase (Nd_8Fe_(27)B_(24)) prior to α-Fe and Nd_2Fe_(14)B phases is crystallized as the amorphous Nd_(3.6)Pr_(5.4)Fe_(83)Co_3B_5 is heated to 1 223 K. The crystallization activation energy of α-Fe and Nd_8Fe_(27)B_(24) phases is larger at the beginning stage of crystallization, and then it decreases with crystallized fraction x for the former and has little change when x is below 70% for the latter, which essentially results in an α-Fe/Nd_2Fe_(14)B microstructure with a relatively coarse grain size about 20-60 nm and a non-uniform distribution of grain size in the annealed alloy. The α-Fe/Nd_2Fe_(14)B nanocomposite magnets with a small average grain size about 14 nm and a quite uniform grain size distribution were prepared by controlled melt-solidification of (Nd_(3.6)Pr_(5.4)Fe_(83)Co_3B_5) at a wheel speed of 20 m·s~(-1) during melt-spinning. The magnets show a high maximum energy product of (BH)max = 194 kJ·m~(-3), which is nearly twice of that of the nanocomposite magnets made by annealing the amorphous Nd_(3.6)Pr_(5.4)Fe_(83)Co_3B_5 precursor alloy. The crystallization kinetics of amorphous (Nd_ (3.6) Pr_ (5.4) Fe_ (83) Co_3B_5) and the preparation of α-Fe / Nd_2Fe_ (14) B nanocomposite magnets by controlled melt-solidification of Nd_ (3.6) (83) Co_3B_5) was investigated by employing DTA, XRD, and TEM. The results show that a metastable intermediate phase (Nd_8Fe_ (27) B_ (24)) prior to α-Fe and Nd_2Fe_ (14) B phases is crystallized as the amorphous Nd_ (3.6) Pr_ (5.4) Fe_ (83) Co_3B_5 is heated to 1 223 K. The crystallization activation energy of α-Fe and Nd_8Fe_ (27) B_ (24) phases is larger at the beginning stage of crystallization, and then it decreases with crystallized fraction x for the former and has little change when x is below 70% for the latter, which essentially results in an α-Fe / Nd 2 Fe 14 microstructure with a relatively coarse grain size about 20-60 nm and a non-uniform distribution of grain size in the annealed alloy. The α-Fe / Nd 2 Fe 14 B nanocomposite magnets with a small average grain size about 14 nm and a quite unif orm grain size distribution were prepared by controlled melt-solidification of (Nd_ (3.6) Pr_ (5.4) Fe_ (83) Co_3B_5) at a wheel speed of 20 m · s ~ high maximum energy product of (BH) max = 194 kJ · m -3, which is nearly twice of that of the nanocomposite magnets made by annealing the amorphous Nd_ (3.6) Pr_ (5.4) Fe_ (83) Co_3B_5 precursor alloy .