Abstract
The preparation route has been shown to have a significant influence upon the catalytic behaviour of Ni2Mo3N samples for ambient pressure ammonia synthesis. Materials prepared from a NiMoO4 precursor necessarily contain a significant fraction of Ni impurity phase. Materials prepared from this precursor are relatively inactive for ammonia synthesis, whereas Ni2Mo3N of much greater phase purity and catalytic activity can be prepared from precursors employing a modified Pechini method with the use of citrate gels. Ni2Mo3N can be prepared by N2/H2 pre-treatment which represents a significant advantage over routes employing ammonolysis. Bulk lattice nitrogen appears to be relatively unreactive in Ni2Mo3N, although heterolytic nitrogen isotopic exchange studies indicate that a significant degree is exchangeable subject to pre-treatment conditions. The modified Pechini method based route has also been shown to be applicable to the preparation of CoNiMo3N of relatively high phase purity, thereby allowing access to the preparation of quaternary nitrides for catalytic screening.
Highlights
Metal nitrides have attracted interest as catalysts for a range of reactions [1,2,3,4]
The powder X-ray diffraction patterns and the surface areas and nitrogen contents of the two materials prepared by ammonolysis and N2/H2 pre-treatment of the NiMoO4 precursor are presented in Fig. 1 and Table 1, respectively
Ambient pressure ammonia synthesis testing has been undertaken with both the samples which have been found, consistent with previous observations [12], to exhibit very low activities in view of literature indicating Ni2Mo3N materials to be active catalysts, and the observation that it seems possible to form this phase by direct application of N2/H2 which would be of greater interest than ammonolysis for large scale application, the role of preparation method has been investigated in more detail
Summary
Metal nitrides have attracted interest as catalysts for a range of reactions [1,2,3,4]. The powder X-ray diffraction patterns and the surface areas and nitrogen contents of the two materials prepared by ammonolysis and N2/H2 pre-treatment of the NiMoO4 precursor are presented in Fig. 1 and Table 1, respectively.
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