By varying various experimental conditions such as heating rate, molar hourly space velocity (MHSV), and nitridation reaction temperature, vanadium oxynitride was prepared through temperature programmed reduction/ nitridation reaction (TPRN) of vanadium pentoxide and ammonia, and characterization were performed. In order to investigate the physico-chemical properties of the prepared catalyst, N2 adsorption-desorption analysis, X-ray diffraction analysis (XRD), hydrogen temperature programmed reduction (H2-TPR), temperature programmed oxidation (TPO), ammonia temperature programmed desorption (NH3-TPD), transmission electron microscopy (TEM) was performed. Transformation of V2O5 with 5 m2 g-1 low specific surface area by reduction at 340℃ to V2O3 showed a high specific surface area value of 115 m2 g-1 by micropore formation. As the nitridation temperature increased beyond that, the specific surface area continued to decrease due to sintering. The nitridation reaction variable that had the greatest influence on the specific surface area was the reaction temperature, and the x + y value of VNxOy of a single phase approached from 1.5 to 1.0 as the nitridation reaction temperature increased. At a high reaction temperature of 680℃, the cubic lattice constant a was VN. close to the value. At 680℃, the highest nitridation temperature among the experimental conditions, the ammonia conversion rate was 93%, and no deactivation was observed.