Syntesis of Niobium Nitride Using Cryogenic Milling

Abstract

In the present paper a preliminary study was performed on the influence of mechanical milling on the synthesis of niobium nitrade. The niobium metal powder sample, passing # 635 mesh sieve, was processed by mechanical milling in SPEX mill for 8 hours using a ball-to-powder ratio of 7:1 and a nitrogen atmosphere. The powder was annealed at different temperatures, 900 °C, 1000 °C, 1100 °C and 1200 °C for 1 hour in a hydrogen and argon atmosphere to study their crystallization, which then were formed into blanks for analysis of the compressibility curves. These samples were also subjected to X-ray diffraction and the data were compared between the annealing temperatures. The compressibility curves of niobium samples with and without grinding were also evaluated, showing high compacting capacity. These samples were subjected to X-ray diffraction and X-ray fluorescence. As the formation of nitrides (Nb2N) was observed in SPEX type mill, the interest in studying the synthesis of nitrides came up, using mechanical milling in Attritor type mill. Same previous results of Attritor processing indicate a Nb2N and NbN synthesis after annealing treatments.