A vanadium nitride alloy can be used as an alloying source of nitrogen and vanadium elements in high-strength steel. In this study, comprehensive and systematic experiments were conducted to optimize the process conditions for producing a vanadium nitride alloy from the starting materials (V2O5 and Fe2O3). The reduction and nitridation behaviors of the starting materials were investigated using thermogravimetry-differential scanning calorimetry (TG-DSC) and horizontal tube furnace experiments under various gas conditions. The phase and chemical compositions of the final alloy products were analyzed using X-ray diffraction (XRD), scanning electron microscope-electron dispersive spectroscopy (SEM-EDS), and the inert gas fusion (IGF) technique. In addition, thermodynamic calculations were performed to help in the understanding of the Nitrovan production process.