Synthesis of Niobium Nitride

S. Zhang and Z. A. Munir, The combustion synthesis of refractory nitrides Part II, the synthesis of niobium nitride, J. Mater. Sci. 1991, 26, 3380-3385. 

Yeh, CL. and Chuang, H.C. (2004) Experimental studies on self-propagating combustion synthesis of niobium nitride. Ceram. Int, 30 (5), TSi-l S. 

Synthesis of Niobium Nitride by Combustion of Ferroniobium in Nitrogen... 

Scheme 5.11 Cleavage of dinitrogen in the synthesis of niobium nitride complex.

Green and co-workers (68) prepared 5-NbC with surface areas as high as 113 m /g from the TPRe of niobium oxide with C2H6/8.6 H2 as a reactive gas. They also synthesized 5-NbC with a surface area of 76 m /g from the carburization of niobium nitride using CH4/4H2 mixture gas. They did not report the elemental analysis data for these materials, which would give information on the carbon contamination. In most cases, the use of the nitride as a precursor or ethane as a reactant increases the surface area of the products, as well as lowers the required synthesis temperature. Nitrides can be converted readily to carbides while maintaining both the high surface area and structure. 

T Tsuchida, Y Azuma. Synthesis of niobium carbide and nitride in air from mechanically activated Nb-C powder mixtures. J Mater Chem 7 2265, 1997. 

Combustion Synthesis of Nitrides of Vanadium, Niobium, and Tantaium... 

Linde, A.V., Grachev, V.V., and Marin-Ayral, R.M. (2009) Self-propagating high-temperature synthesis of cubic niobium nitride under high pressures of nitrogen. Chem. Eng. J., 155, 542-547. 

Djega-Mariadassou and co-workers (67) reported that a long induction period preceded the simultaneous reduction and carburization steps in the synthesis of NbC from the TPRe of niobium oxide with CH4/4H2. To avoid the long induction period, different catalysts were incorporated into the initial Nb205 and were treated with CH4/4H2 mixtures at relatively low carburization temperatures. In the presence of catalysts of methane decomposition (Ni and Rh), they were able to eliminate the induction period and fee 5-NbC with superficial carbon contamination and surface areas of 11-18 m /g were obtained. When a NiMo catalyst was mixed with Nb205 and carburized with a CH4/4H2 mixture gas, 5-NbC with a surface area of 50 m /g and large amounts of carbon contamination was produced. They also synthesized 5-NbC with surface areas of 27-49 m /g from the carbonization of niobium oxynitrides, which were prepared from the nitridation of niobium oxide with pure ammonia at 923 K. 

Akagi P, Suzuki S, Ishida Y, Hatanaka T, Matsuo T, Kawaguchi H. Reactions of a niobium nitride complex prepared from dinitrogen synthesis of imide and ureate complexes and ammonia formation. Eur J Inorg Chem. 2013 3930—3936. 

T Wade, RM Crooks, EG Garza, DM Smith, JO Willis, JY Coulter. Electrochemical synthesis of ceramic materials. 3. Synthesis and characterization of a niobium nitride precursor and niobium nitride powder. Chem Mater 6 87, 1994. 

This chapter presents a review of the synthesis of vanadium, niobium, and molybdenum carbides and nitrides by the TPR method. Factors responsible for development of surface area during transformation are discussed. 

Antonelli and co-workers have recently demonstrated that room temperature stoichiometric ammonia synthesis is possible with their mesoporous titanium and niobium oxide catalysts. In this study, they proposed that the ammonia species are formed via the reaction activated nitrogen with the underlying moisture of the support. Reversible, inter-conversion of and NH2 species via exposure to moist air for aluminophosphate oxynitride catalysts has been observed by FTIR and XPS by Marquez and co-workers. There has been a lot of interest in the literature in the development of novel routes for the low temperature stoichiometric conversion of nitrogen to ammonia, e.g.. However, in principle this could be realised by the nitridation of Li, followed by hydrolysis, although the kinetics would be very slow. 

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