Fe75Zr3Si13B9 magnetic amorphous powders were fabricated by mechanical alloying. Bulk amorphous and nanocrystalline alloys with 20 mm in diameter and 7 mm in height were fabricated by the spark plasma sintering technology at different sintering temperatures. The phase composition, glass transition temperature (Tg), onset crystallization temperature (Tx), peak temperature (Tp) and super-cooled liquid region (ΔTx) of Fe75Zr3Si13B9 amorphous powders were analyzed by X-ray diffraction (XRD) and differential scanning calorimetry (DSC). The phase transition, microstructure, mechanical properties and magnetic performance of the bulk alloys were discussed with X-ray diffractometer, scanning electron microscope (SEM), Gleeble 3500 and vibration sample magnetometer (VSM), respectively. It is found that with the increase in the sintering temperature at the pressure of 500 MPa, the density, compressive strength, micro-hardness and saturation magnetization of the sintering samples improved significantly, the amorphous phase began to crystallize gradually. Finally, the desirable amorphous and nanocrystalline magnetic materials at the sintering temperature of 863.15 K and the pressure of 500 MPa have a density of 6.9325 g/cm3, a compressive strength of 1140.28 MPa and a saturation magnetization of 1.28 T.