Nanostructured niobium nitride was synthesized through a solid-gas reaction in an atmosphere of nitrogen and hydrogen using an oxalic niobium precursor. Crystal phases evolution throughout the reactive processes were evaluated using X-Ray Diffraction, reaction parameters modifications were performed in isotherm time, gas flow, and precursors' mass. It was verified the synthesis of a stable NbN material with a hexagonal structure under the following conditions: 1g of precursor, 300 min of isotherm at 1100 °C and, the gas flow of N 2 = 40% (v/v), and H 2 = 60% (v/v). The increase in gas phase flow and the decrease of solid load favored the process, and a pure and single-phase powder was obtained. This set indicates the importance of physical resistance in the fluid-particle interaction process. Under these conditions, the solid obtained had a crystallite size of 30 -50 nm.