The microstructural change of the Ni-19Si-3Nb-0.15B alloys after different heat treatment was examined by scanning electron microscopy with energy dispersive spectrum. In addition, Vickers's hardness test was used to measure the variation of mechanical properties for each heat-treated alloy. The results reveal that the typical dendritic microstructure of the heat-treated alloys (comprised of dendritic β-phase, α-β eutectic, and the Nb-rich precipitates) remained almost the same microstructure as the as-cast alloy. However, the morphology of the sharp-edged Nb-rich precipitate (identified to be the cubic Nb3Ni2Si by electron diffraction of TEM) would be blunted by homogenization. In addition, the size of precipitates seemed to grow with increased aging temperature and aging time. Correlating the result of microhardness measurement with the microstructure observation, an aging temperature of 700 °C and an aging time of 10 h is found to be the optimum treating condition for the Ni-19Si-3Nb-0.15B alloy. In addition, the precipitate growth is revealed dominating by an interfacial-controlled kinetics with a thermal activation process of Arrhenius type. The strengthening effect of the heat treatment is not obvious from the hardness test. However, the effect of heat treatment exhibited significant improvement on the ductility of the Ni-19Si-3Nb-0.15B alloy (ε ∼3% for as-cast alloy and 12% for heat-treated alloy).