Study and analysis of NbN and TaN synthesis parameters via gas-solid reaction
Gas-solid reaction, X-ray diffraction, niobium nitride, hexagonal phase, tantalum nitride, granulometry.
In order to adapt the advancement of technology along with economic growth, new ideas arise for the use of clean energy sources. The studies of new materials have been gaining ground to improve their properties and their performance in the face of their applications. Currently, the development of new methods, processing and compositions have been invested in order to optimize the processes, as well as obtain low cost and less energy expenditure. Niobium and tantalum nitrides are nanocrystalline materials that have good electronic conductivity, high melting point, wear resistance, superconducting properties, among other properties, make these materials promising for many technical applications, including aerospace, capacitor production and anticorrosive materials. Among the various synthesis methods, the gas-solid reaction route has advantages, such as ease of operation, low maintenance cost and shorter processing time, in addition to allowing the control of crystallite size. In this article, niobium and tantalum precursors were used for the synthesis of nitrides, since these precursors have more reactivity than niobium and tantalum oxides. The materials obtained were characterized by XRD, Rieltveld refinement, SEM/FEG, HRTEM, granulometry and crystallite size calculation. Niobium nitride was synthesized through the precursor niobium oxalate under conditions of 1100 ºC with a flow rate of 44.7 L/h and an isotherm of 300 min and the NbN phase with hexagonal structure and absence of impurities was obtained. From the study of tantalum nitride synthesis parameters, it was observed that the variation in the granulometry of the tantalum oxalate precursor influenced the obtaining of the sample with the highest presence of the Ta5N6 phase with hexagonal structure. The synthesis conditions were more effective to obtain pure niobium nitride, while for tantalum nitride, more synthesis conditions must be studied to optimize the process of obtaining the desired material.