Ammonia is one of the most critical chemical commodities produced and is integral to a number of current industries such as agriculture as well as a key part to future sustainability areas such as clean H2 production. However, the current production methods for ammonia are largely unsustainable and produce large amounts of CO2 emissions. This combined with the current dependence on fossil energy for production has led to researchers attempting to develop a clean and sustainable method for ammonia production. This method involves the thermochemical looping of a nitride compound with H2, and the renitridation of the compound with N2. This thermochemical loop would significantly reduce pressure requirements for ammonia production in addition to only being reliant on renewable inputs. This paper expands and complements this research by detailing the methods for the synthesis of nitride compounds as well as confirming their structure through material characterization. The nitride compounds as well as their oxide precursors were synthesized through Pechini synthesis and co-precipitation, and their structure was confirmed through the use of X-ray diffraction analysis. The XRD patterns of the synthesized nitrides matched those previously synthesized as well as those found in literature. In addition, observation of the spectra for the oxide CoMoO4 showed a marked similarity to that of the oxide precursor for (NixCox)2Mo3N. However, further testing is necessary regarding the phase-purity of synthesized nitrides, as well as the reduction and renitridation capability of nitrides in the line of (NixCox)2Mo3N.

Ammonia is one of the most important chemicals for modern civilization as well as a potentially invaluable intermediary component of a future sustainable H2 economy, yet its current production is decidedly unsustainable. Accordingly, researchers are attempting to devise new paradigms for ammonia production, one of which would involve the cyclical reaction of H2 with a nitride compound and the renitridation of that compound with N2 - a thermochemical loop that would allow for ammonia production with renewable inputs and at relatively low pressures. In this paper, researchers identified several ternary and quaternary metal nitrides with the potential to exhibit relatively favorable thermodynamics for both the reduction and nitridation steps of that reaction cycle. These compounds were synthesized via co-precipitation and Pechini synthesis and several were tested under gas flows of 75% H2/Ar at 100-700 C and 75% H2/N2 at 700 C to determine their behavior under these conditions. As suggested by the available literature, Co3Mo3N was found to be a far better candidate for thermochemical looping than Fe3Mo3N or Ni2Mo3N - with higher mass loss and mass regain. Interestingly, quaternary nitrides containing Fe and Co in addition to Mo also demonstrated remarkable reduction and nitridation capability under ambient pressures. Ultimately, this paper demonstrates the feasibility of synthesizing a variety of single phase ternary and quaternary nitrides and the potential that several of these nitrides hold for producing ammonia sustainably via cyclic thermochemistry.