β-FeSi₂ was successfully produced by making use of the combined process of mechanical alloying (MA) and spark plasma sintering (SPS). The MA was perforomed under the Ar gas atomsphere using mixed powders of pure iron and silicon having the mole fraction of 1: 2. The SPS process was performed at 1073 K with the heating rate of 1.33 K/s and the holding time was ranging from 0 to 15 ks. The combined process was quite effective for the production of β-FeSi₂, where the minimum SPS time required was found to depend on the MA time. The shortest SPS holding time of Os was achieved for the powders mechanically alloyed for 72ks.
The relative density of each sinter is around 90% (4.44g/cm³) to its ideal density, and especially the density of 97.4% was obtained for the sinter which was mechanically alloyed for 72ks, followed by the SPS treatment for 600s.