Changes in the phase composition and crystallite size, as well as changes in the magnetic behaviour of Nd 4.5 Fe 77 B 18.5 alloy, caused by thermomagnetic measurements, was observed in regard of the optimal magnetic state of this alloy. In the optimized magnetic state, the formed nanocomposite consisted of Fe3B/Nd2Fe14B and partly of α-Fe with a mean crystallite size < 30 nm, as determined by X-ray diffraction and transmission electron microscopy. An increased amount of α-Fe, the presence of Nd 2 O 3 and different Fe-B phases, as well as an increase in the mean crystallite size were observed after thermomagnetic measurements had caused a quality loss of the hard magnetic properties.