This present study revealed the synthesis and heating rate effect on the mechanical attributes of spark plasma sintered NiAl intermetallic compound. The milled specimen was consolidated by field assisted sintering technique (SPS), morphology of the specimens was determined using the scanning electron microscope. The microstructures of the sintered NiAl that was carried out between the heating rates of 50 to 150 °C/min showed the presence of micro pores. The hardness value (Vickers microhardness) of the specimens was found to increase while the heating rate increases. Furthermore, highest hardness value of 555.4 HV0.1 was recorded for the sintered pellet possessing the heating and cooling rate of 150 °C/min. In addition, the densification of the sintered specimen (150 °C/min heating rate) was measured as 96.2%.