A powder metallurgical process has been applied to synthesize the FeNiCr+Y2O3 oxide dispersion strengthened (ODS) alloys. The composition of the reinforcing Y2O3 added into matrix was varied from zero to 2.0 percent weight. Raw powders were carefully weighed with a four-digit balance. Y2O3 powder was pre-linked into Fe powder as the dominant element in the matrix by manually ground for half an hour. Ni and Cr powders were then mixed evenly for the next a half hour to obtain FeNiCr+Y2O3 precursor. Avoiding agglomeration and grain coarsening, the precursor was uniformly homogenized by milling for 20 hours. The precursors were then compressed at an isostatic pressure of 100 kN to 12 grams of pellets each. To prevent sample erosion during smelting with an electric arc furnace (EAF), crystal growing mechanism by conventional sintering was performed at 900 °C for 2 hours. This strengthens the bonds between precursors in forming ODS alloys. The samples were then melt-casted in the arc by 4 times flips. As a result, the neutron diffraction analysis and SEM-EDS strongly reveal the austenitic crystal structure and Y2O3 oxide successfully dispersed in the cast-alloy respectively. The microstructures with Y2O3 oxide spread uniformly overall the cast-alloy surfaces.