From the viewpoint of fundamental study of steelmaking, the direct determination of the structure and composition of niobium nitride in equilibrium with liquid Fe-Nb-N alloy has been attempted by means of high temperature X-ray diffraction technique. X-ray analysis has also been carried out at room temperature for niobium nitride powder extracted from the solidified alloy ingot.It was found from a high temperature X-ray diffraction pattern that the niobium nitride equilibrating with liquid Fe-(11.5-14.3) mass%Nb-N alloy at 1813 K under an atmospheric pressure of nitrogen 14.3) mass%Nb-N alloy seemed to be morphologically invariant during the cooling and solidification at the rate of 3-5K/s or 0.2-0.5K/s.The lattice parameter of niobium nitride was determined to be 0.4385nm at room temperature, and its composition was estimated to be Nb1 .1N from the relation between the lattice parameter and the ratio N/ Nb. Provided that the composition of niobium nitride does not change in the course of cooling and solidification, the niobium nitride forming reaction in liquid Fe-(11.5-14.3) mass%Nb-N alloy at 1813 K under an atmospheric pressure of nitrogen is expressed as follows:1.1Nb+N=Nb1.1N(s).