Bulk Fe75Nb3Si13B9 amorphous and nanocrystalline alloy with 10mm in diameter and 6mm in height was fabricated by mechanical alloying and spark plasma sintering technology.The phase composition, glass transition temperature (Tg), onset crystallization temperature (Tx), peak temperature (Tp) and super-cooled liquid region (△Tx) of Fe75Nb3Si13B9 amorphous alloy powders were analysed by X-ray diffraction and differential scanning calorimetry.The phase transition, microstructure, mechanical properties, resistivity and magnetic properties of the bulk alloys at different sintering temperatures were discussed by X-ray diffraction, scanning electron microscope, transmission electron microscope, Gleeble 3500, power conversion efficiency measuring instrument and vibration sample magnetometer, respectively.It is found that with the increase of the sintering temperature at the loading pressure of 500MPa, the density, compressive strength, micro-hardness and saturation magnetization of the sintering samples were improved significantly, the amorphous phase gradually began to crystallization.Finally, the desirable amorphous and nanocrystalline magnetic materials under the loading pressure of 500MPa at the sintering temperature of 883K has a a density of 6.604 g/cm3, compressive strength of 1196.45MPa and a saturation magnetization of 156.11emu/g.